United States Environmental Protection Agency Office of Pollution Prevention and Toxics EPA 747-R-98-008 October 1998 Lead-Cleaning Efficacy Follow-Up Study ------- October 1998 EPA747-R-98-008 Lead-Cleaning Efficacy Follow-Up Study Technical Branch National Program Chemicals Division Office of Pollution Prevention and Toxics Office of Prevention, Pesticides, and Toxic Substances United States Environmental Protection Agency Washington DC 20460 ------- DISCLAIMER This document has been prepared for the Office of Pollution Prevention and Toxics (OPPT), U.S. Environmental Protection Agency. The material in this document has been subject to EPA technical and policy review and approved for publication as an EPA report. The use of trade names or commercial products does not constitute Agency endorsement or recommendation for use. ------- CONTRIBUTING ORGANIZATIONS The study described in this report was funded by the United States Environmental Protection Agency (EPA). The study was managed by EPA and conducted by Midwest Research Institute (MRI) with the assistance of Westat, Inc., under contract to EPA. Each organization's responsibilities are listed below. Midwest Research Institute (MRI) MRI, assisted by Westat, Lie., worked with EPA to design this follow-up study to a previous EPA study performed jointly by Westat and MRI. MRI then conducted all laboratory sampling and chemical analyses. Upon completion of the laboratory activities, MRI performed the statistical analysis and prepared and edited the report Westat, Inc. Westat, Inc., assisted MRI in the development of the experimental design based on the results from the previous study and EPA's requirements for this follow-up study. United States Environmental Protection Agency EPA was responsible for managing the study; providing technical oversight, guidance and direction; and overseeing the peer review and finalization of the report. Dr. Benjamin S. Lim was the Work Assignment Manager for this task, and the EPA Project Officer was Mr. Samuel F. Brown. ------- Executive Summary In the past, the U.S. Environmental Protection Agency (EPA) recommended the use of trisodium phosphate (TSP) detergent to clean lead-contaminated dust from surfaces after residential lead hazard control work to achieve post-abatement clearance standards. This recommendation was often assumed to apply to the general cleaning of lead-contaminated dust during ongoing exposure reduction activities. Because of the negative impact of phosphate detergents on the ecology of aquatic ecosystems, questions arose as to the scientific basis for recommending TSP and about the effectiveness of other cleaners. In 1996, an EPA study was conducted to determine the relative effectiveness of many commercially available cleaners for cleaning lead-contaminated soil from surfaces similar to floors and walls. The results of that study, to be used to support EPA's recommenda- tions to the public on methods for removing lead-contaminated dust and soil from surfaces, are published in the EPA report entitled "Laboratory Study of Lead-Cleaning Efficacy," publication No. EPA-747-R-97-002, March 1997.1 That study was designed to determine if and how cleaner characteristics such as pH, phosphate content, surfactant type, and surface tension affect the relative cleaning efficacy as measured by the quantity of lead picked up by a baby wipe after the test surfaces were cleaned. Based on the results reported in the study, it was shown that of the cleaner characteristics tested, only surface tension appeared to be related to how well the cleaners cleaned the lead-containing soil from the surfaces; cleaners with lower surface tensions appeared to clean the surfaces slightly better than cleaners with higher surface tension. However, surface tension was a measured cleaning agent property, not a controlled variable. The results from this previous study provided only weak evidence for the selection of a cleaning detergent for the purpose of cleaning lead-contaminated dust from surfaces in homes. By design and availability, the commercially available cleaners used in the previous study covered only a narrow range of surface tension and phosphate content. The EPA thus sponsored a follow-up study to further investigate the effect of surface tension and phosphate content on lead-cleaning efficacy. This follow-up study consisted of the selection of a commercially available hand dishwashing detergent to assess the effect of surface tension on lead-cleaning efficacy of a standard sponge-cleaning procedure. Four surface tensions, 30,40,60, and 70 dyne/cm, were approximated by mixing the four amounts of cleaning agent of 6.36,0.050,0.008, and 0 g, respectively, into 1 gallon of water. Additionally, the effect of phosphate content on lead-cleaning efficacy was investigated by adding known amounts of anhydrous trisodium phosphate to the cleaning solutions corresponding to concentrations of 0, 3,11, and 14 grams of phosphorus per gallon (g P/gal). This design provided 16 cleaning solutions to be tested. Tests were conducted using two types of surfaces—enamel-painted birch plywood and latex-painted birch plywood—each one foot square (called coupons). Two types of soil ------- were used: one contained some vegetable oil, the other, a dry soil, contained no added oil. A total of 128 coupons were soiled then cleaned with a sponge containing the cleaning solution. Half the coupons were then wiped with a commercially available, pre-wetted baby wipe, the other half were not. All coupons were then cored to obtain coupon samples. All sponges, wipes, and core samples were analyzed by ICP and GFAA, if necessary, for lead content. The percentage of lead removed by the sponge and the wipe and that remaining on the coupon was statistically analyzed to quantify the effect, if any, of surface tension and phosphate content, on the cleaning efficacy of the various cleaning solutions. Based on the 128 sponge-cleaning tests, 64 wipe tests, 64 coupon tests from wiped surfaces, and 64 coupon tests from 64 non-wiped surfaces, the following conclusions were drawn. • Approximately 72 to 74 percent of the lead applied was removed by the sponge. • Approximately 1.3 to 1.6 percent of the lead applied was removed by the wipes after the surfaces were cleaned by the sponge. Approximately 20 to 23 percent of the lead applied remained on the coupons after sponge-cleaning and wiping. • Approximately 22 to 26 percent of the lead applied remained on the coupons after sponge-cleaning only. • The total percentage of lead accounted for in this study was estimated at approximately 95 to 99 percent, leaving approximately 0.9 to 5.3 percent unaccounted for. The amount of lead picked up by the wipe from the sponge-cleaned surface was estimated at approximately 2 percent in the previous study. This estimate is comparable to the slightly lower estimate of 1.3 to 1.6 percent found in mis study. In contrast, the estimated amount of lead remaining on the cleaned surface, expressed in percentage of applied amount, is significantly higher in this study than in the previous study: 20 to 26 percent versus 7 percent. The estimate of 20 to 26 percent was directly estimated from cleaning tests in this study. Since neither sponges nor surface samples were analyzed in the previous study, the percentage of lead removed by a cleaner and sponge was based on a small set of wipe cleaning experiments. In that study, the assumption was made that two baby wipes would remove similar quantities of lead as would a cleaner and sponge. That estimate was found to be roughly 91 percent. By subtraction, the percentage of lead remaining on a cleaned and wiped surface was estimated at 100 percent - 91 percent - 2 percent = 7 percent. VI ------- The analysis of the effect of surface tension and phosphate content on cleaning efficacy provided the following results: • Overall, surface tension and phosphate content had no statistically significant effect on the residual lead found on coupons. This is true whether the coupons were wiped or not after sponge cleaning. • When sponge and wipe results were examined, both surface tension and phosphate content had an overall statistically significant effect on cleaning efficacy. However, no consistent pattern in the effect of these two factors on cleaning efficacy could be found. That is, no monotonic relationship could be found between the levels (values) of these factors and the resulting cleaning efficacy. This lack of consistent pattern was found in sponges and wipes. For example: - Across all coupon surface types, soil types, and phosphate content levels, it was found that lower surface tension cleaning solutions are associated with better sponge cleaning. However, this significant surface tension effect is masked by interactions with the type of coupon surface and soil type. When looking individually at the four combinations of surface type and soil type, surface tension was no longer predicting cleaning efficacy when using a sponge. - Only when dry soil was applied to latex-painted surfaces did phosphate content affect cleaning efficacy when a sponge was used. However, no meaningful relationship between cleaning efficacy and phosphate content level could be found. In other words, cleaning efficacy did not increase or decrease consistently with phosphate content. - Surface tension had a small but significant effect on the ability of wipes to pick up lead from all surfaces. It was found that the percentage amount of lead picked up by the wipe increased with increasing surface tension of the cleaning solution. The effect of surface type and soil type on cleaning efficacy was also investigated. The analysis provided the following results: • Surface type (enamel- and latex-painted plywood surfaces), soil type (dry and oily), and their interaction had in most cases a significant effect on lead cleaning efficacy. Although latex-painted surfaces are rougher than enamel-painted surfaces, the percentage of lead found in the sponge did not reflect that fact. However, wipes picked up a higher percentage lead from latex-painted surfaces than from enamel- vii ------- painted surfaces after sponge-cleaning, possibly indicating that rougher surfaces are more difficult to clean. • The above finding could not be confirmed when looking at the residual lead on the coupons. In those cases (wiped and non-wiped coupons), the trend was counter-intuitive in that a higher residual lead was found on enamel- (smooth) than latex- (rough) painted surface. • Generally, an oily soil surface was more difficult to clean than a dry soil surface. Based on this study, no conclusive evidence was found to recommend trisodium phosphate (TSP) or high phosphate detergent cleaners for lead removal inside homes. In addition, the weak evidence found in the previous study that cleaners with lower surface tension appear to clean soiled surfaces slightly better than cleaners with high surface tension could neither be refuted nor strengthened. However, EPA still recommends that either a general all-purpose cleaner or a cleaner made specifically for lead should be used for both general cleaning and for post-intervention cleaning. Household cleaning using one of these cleaning agents is likely to remove more leaded soil and dust than does water alone. The extent to which these conclusions, based on laboratory investigation, apply to homes in real-life situations is a matter of judgment. Cleaning home interiors with a damp sponge or cloth will likely remove significant amounts of lead-containing soils. Water alone would do an adequate job, but considering that most cleaning is done by repeatedly wiping a soiled surface and rinsing the sponge or cloth into a bulk cleaning solution, a common household cleaner would probably help keep the soil in suspension, thus lessening the redeposition of the soil back onto the surface being cleaned. General home cleaning will thus further assist in the prevention of childhood lead poisoning. vin ------- Appendices Appendix A—Test Schedule Appendix B—Laboratory Data—Test and QC Samples ------- Appendices Appendix A—Test Schedule Appendix B—Laboratory Data—Test and QC Samples ------- Figures Figure 2-1. Distribution of Percentage of Lead Found in Sponges, Wipes, and on Coupons (Wiped and Not Wiped), by Surface and Soil Types (Log-scale) 2-2 Figure 4-1. Diagram of Soil Application Procedure 4-3 Figure 4-2. Diagram of Core Hole Locations on Coupon 4-4 Figure 5-1. LCS Percent Recovery Control Chart 5-5 Figure 5-2. SRM Percent Recovery Control Chart 5-6 Figure 6-1. Differences Between Nominal and Measured Surface Tension Levels ... 6-3 Figure 6-2. Relationship Between Cleaning Solution Concentration (Log Scale) and Surface Tension 6-5 Figure 6-3. Distribution of Precleaning Lead Concentrations by Soil and Sample Types 6-8 Figure 7-1. Mean Cleaning Efficacy of Sponges versus Phosphate Content When Used on Latex-Painted Coupons Soiled with Dry Soil 7-4 Figure 7-2. Percent Lead Removed by Sponge Versus Surface Tension, Separately by Substrate and Soil Type 7-6 Figure 7-3. Mean Cleaning Efficacy of Wipes Versus Phosphate Content 7-8 Figure 7-4. Mean Cleaning Efficacy of Wipes Versus Surface Tension, Separately by Substrate and Soil Types 7-10 Figure 7-5. Residual Lead Remaining on Coupons After Sponge Cleaning and Wiping Versus Surface Tension, Separately by Substrate and Soil Type 7-12 Figure 7-6. Residual Lead Remaining on Coupons After Sponge Cleaning Only Versus Surface Tension, by Substrate and Soil Types 7-15 Figure 7-7. Total Percentage of Lead Accounted for Versus Surface Tension, by Substrate and Soil Types 7-18 XI ------- Tables Table 3-1. Number of Cleaning Solutions Tested for Each Combination of Phosphate Content and Surface Tension 3-2 Table 3-2. Test Schedule of Proposed Precleaning Tests 3-4 Table 3-3. Test Schedule of Blank Soil Tests 3-4 Table 3-4. Summary of Field Samples Generated 3-5 Table 4-1. Type and Number of Samples by Analytical Method 4-7 Table 5-1. Laboratory Control Sample Results by Matrix 5-4 Table 5-2. Standard Reference Material Results by Matrix 5-7 Table 5-3. Matrix Method Blank Sample Results by Matrix 5-7 Table 6-1. Phosphate Content and Surface Tension Statistics 6-2 Table 6-2. Precleaning Sample Lead Results 6-7 Table 7-1. Analysis of Co variance Results: Cleaning Efficacy of Sponges 7-3 Table 7-2. Mean Cleaning Efficacy of Sponges by Phosphate Content When Used on Latex-Painted Coupons Soiled with Dry Soil 7-4 Table 7-3. Regression Statistics of Percent Lead Removed by Sponge versus Surface Tension (Nonsignificant Results) 7-5 Table 7-4. Analysis of Covariance Results: Cleaning Efficacy of Wipes 7-7 Table 7-5. Mean Cleaning Efficacy of Wipes, Separately for Phosphate Content, Substrate Type, and Soil Types 7-8 Table 7-6. Analysis of Variance Results: Residual Lead on Coupons After Cleaning with Sponge and Wipe 7-11 Table 7-7. Residual Lead on Coupons After Cleaning with Sponge and Wipe by Substrate and Soil Type 7-11 Table 7-8. Analysis of Covariance Results: Residual Lead on Coupons After Cleaning with Sponge Only 7-13 Table 7-9. Residual Lead on Coupons After Cleaning with Sponge Only by Substrate 7-14 Table 7-10. Analysis of Covariance Results: Total Lead Accounted for in the Cleaning Process 7-16 Xll ------- Section 1 Introduction ^ 1.1 Background In the past, the United States Environmental Protection Agency (EPA) recommended the use of trisodium phosphate (TSP), a high-phosphate detergent, to clean lead- contaminated dust from surfaces, both as a general practice and after remediation of lead- based paint. The recommendation to use TSP was often assumed to cover the general cleaning of lead-contaminated dust during exposure reduction activities. Lead- contaminated dust can result from deteriorated or disturbed lead-based paint, lead- contaminated soil and street dust, or other sources. Because of the negative impact of phosphate on the ecology of aquatic ecosystems, questions arose as to the scientific basis of its recommended use and about the effectiveness of other cleaners, in particular, low- phosphate cleaners. 1.2 Summary of Previous Lead-Cleaning Efficacy Study In 1996, an EPA study was conducted to determine the relative effectiveness of different cleaning agents for cleaning lead-contaminated soil from surfaces similar to floors and walls. The results of that study, to be used to support EPA's recommendations to the public on methods for cleaning surfaces with lead-contaminated dust and soil, are published in the EPA report titled "Laboratory Study of Lead-Cleaning Efficacy," publication No. EPA-747-R-97-002, March 1997.1 The objectives of that study were to assess the relative cleaning efficacy of 32 cleaners (commercially available cleaning agents), tap water of average hardness, and TSP as a function of the physical and chemical characteristics of the cleaners. Cleaning efficacy was measured by the quantity of lead (referred to as wipe lead) picked up by a commercially available, pre-wetted baby wipe after the surface had been cleaned. This measure of cleaning effectiveness is used by abatement contractors to assess lead dust cleanup after remediation of lead-based paint. Risk assessors also do wipe sampling of dust to determine if lead hazards are present in a home. The study was designed to determine if and how the following four cleaner character- istics affect the relative cleaning efficacy as measured by the wipe lead: • pH—The measurement of acidity and alkalinity of a solution. Solutions with a pH greater than 7.0 are basic (alkaline); solutions with a pH less than 7.0 are acidic; pure water has a pH of 7.0. 1-1 ------- • Phosphate content—The amount, in grams of phosphorus per gallon of cleaning solution. Various phosphate chemicals have traditionally been added to detergent cleaners to enhance their effectiveness. • Surfactant type—The classification of the surfactant, or wetting agent, in the cleaner. There are four major classifications of surfactants, of which two were considered in this study: anionic and nonionic. Anionic surfactants are water soluble and have negative ions. Nonionic surfactants, a class of synthetic surfactants, are the most widely used for surface cleaning and have no charge. Cleaning solutions with a blend of anionic and non-ionic surfactants types were also included in the study. • Surface tension (dyne/cm)—The force acting on a liquid's surface caused by intermolecular bonding interaction. Surface tension is a measure of how well the cleaning solution will wet the surface to be cleaned: the lower the surface tension of the cleaning solution, the more effectively the cleaning solution will wet the surface. Pure water (without a cleaner) has a high surface tension of 70 dyne/cm. Cleaners, by design, lower the surface tension of water to low values of around 30 dyne/cm. The tests were conducted using five types of surfaces selected to represent those commonly found in residential settings: vinyl tile, latex paint on drywall, enamel paint on birch, lacquer (Fabulon) on oak, and latex paint on birch. In addition to varying the types of surfaces tested, two types of leaded soil were used. One soil type contained vegetable oil (oily soil); the other contained no vegetable oil (dry soil). Each lead-containing soil mixture was dispersed in a mineral spirits carrier, spread on a test surface in a standardized manner, and allowed to dry before the surfaces were cleaned. Based on the results reported in the study, the following conclusions were drawn: 1. Roughly 91 percent of the applied lead is removed by cleaning the surface. 2. Roughly 2 percent of lead is recovered from the baby wipe after cleaning the surface. 3. Therefore, roughly 7 percent of the applied lead remains on the surface. 4. Of the cleaner characteristics tested, only surface tension appears to be related to how well the cleaners cleaned the lead-containing soil from the surfaces; cleaners with lower surface tension appear to clean the soiled surfaces slightly better than cleaners with higher surface tension. However, surface tension was a measured cleaning agent property, not a controlled variable. The results obtained provided only weak evidence for the selection of a cleaning detergent for the purpose of cleaning lead-contaminated dust from surfaces in homes. The 1-2 ------- commercially available cleaners used in the study were selected based on their pH, the type of surfactant, and their phosphate content. However, cleaning agents currently available to the consumer (1) are relatively high in pH for corrosion control of steel machine parts; (2) employ surfactant types, the use of which is based on the profit margin of the cleaning product; and (3) include a phosphate content that is minimized or eliminated due to regulatory and marketing constraints. As a result, there was little latitude to study statistically the effects and interactions of the selected parameters on lead-cleaning efficacy: most of the cleaning agents studied were high in pH, of the anionic and nonionic surfactant type, and low in phosphate content. Furthermore, due to the selection criteria, the cleaning agents tested covered the range of surface tensions from 25 to 50 dyne/cm, with most of the values being below 35 dyne/cm. 1.3 Objectives of Follow-Up Study Based on the statistical results from the previous study and given its limitations, EPA proposed a follow-up study to further investigate the effect of surface tension and phosphate content on lead-cleaning efficacy. Using a single cleaning agent at various dilution levels, with the addition of known amounts of phosphate, a study was thus undertaken to accomplish the following: 1. Determine the lead-removal efficacy of a cleaning agent as a function of its surface tension, covering a range of surface tensions of approximately 30 to 70 dyne/cm. 2. Determine the lead-removal efficacy of a cleaning agent as a function of its phosphate content, covering a range corresponding to approximately 0 to 14 grams of phosphorus per gallon of cleaning agent. 3. Quantify the amount of lead actually removed from the test coupon surface by the sponge-cleaning procedure. This would be accomplished by measuring the lead content of the sponge, cleaning agent, and rinse water from the sponge-cleaning process for individual test coupons. 4. Quantify the amount of lead remaining on the surface of the test coupon. This would be accomplished by measuring the lead content of core samples taken from the substrates. Of the five previously tested substrates, only two, enamel-painted birch plywood and latex-painted birch plywood, were selected. As in the previous study, two types of leaded soil, dry and oily, were used to soil the test coupons. 1-3 ------- 1.4 Overview of the Report • The study results as they apply directly to the objectives are presented in Section 2. A synopsis of the previous lead-cleaning efficacy study is provided in that section also. The study design is described in Section 3. Section 4 describes laboratory data collection procedures for the preparation, soiling, and cleaning of the coupons, and the analytical quantification of lead. Section 5 summarizes the QA/QC results of the study. The characterization of the cleaning solutions and the soil is described in Section 6. Finally, the statistical results are presented in Section 7. Appendices A and B provide supporting analytical data. 1-4 ------- Section 2 Study Summary When lead-based paint/lead-based paint hazards are abated or interim controls are performed in a home, the contractor is required to clean the lead-contaminated dust. A surface is considered clean if the quantity of lead picked up by a baby wipe is below clearance levels. (The clearance levels from Chapter 5, Risk Assessment, of the 403 Guidance are 100 jig/ft2 for carpets and hardwood floors, 500 ug/ft2 for interior window sills, and 800 jig/ft2 for window troughs. Lower clearance levels are presently being proposed that will present even more challenge to the cleaning process.) Risk assessors also perform wipe sampling of dust to determine if lead hazards are present in a home. The same approach was used in this laboratory study. Cleaning solutions that remove most of the lead will leave less lead to be picked up by the wipe. Therefore, for the most effective cleaning solutions, the quantity of lead picked up by a wipe and the quantity of lead remaining on the surface will be less than for other cleaning solutions. Sixteen cleaning solutions were evaluated for their ability to clean two surface types soiled with two soil types. The effect of phosphate content and surface tension, and their interaction on cleaning efficacy was investigated. The percentage of lead removed by the sponge and the wipe and that remaining on the coupon surfaces (either wiped or not) was estimated for various experimental conditions. To be consistent with the terminology of the previous study,1 the lead remaining on the coupon is called residual lead and is expressed as a proportion (or percentage) of the quantity of the lead on the coupon before cleaning. Similarly, the lead captured by the sponge and wipe is expressed as a proportion (percentage) of the lead on the coupon before cleaning. The distribution of these percentages is shown, on the log-scale, in the form of boxplots in Figure 2-1, separately for the four combinations of soil (dry and oily) and surface types (enamel- and latex-painted). [Note: Coupon(O) and Coupon(l) on the X-axis indicate sponge-cleaning only and sponge- cleaning and wiping, respectively.] This section provides an overview of the study design and a discussion of conclusions. 2.1 Design A commercially available hand dishwashing detergent (cleaning agent) was selected to assess the effect of surface tension on lead-cleaning efficacy of a standard sponge-cleaning procedure. (The reasons for choosing a hand dishwashing detergent are discussed in detail in Section 3.2.) The four surface tensions of 30,40,60, and 70 dyne/cm were approximated by mixing the four amounts of cleaning agent of 6.36,0.050,0.008, and 0 g, respectively, into 1 gallon of water. Surface tensions below 25 to 30 dyne/cm are difficult 2-1 ------- ENAMEL.DRY SOIL ENAMEL.OILY SOIL 100.0 I 8 10.0 £ I 1.0 100.0 c XX Sample type LATEX.DRY SOIL 100.0 i. 10.0 £ e xx Sample type S 10.0 * £ § 1.0 XX Sample type LATEX.OILYSOIL 100.0 Pb (%) 10.0 b XX Sample type Legend: coupon(O) indicates that the coupon was not wiped after sponge-cleaning coupon(l) indicates that the coupon was wiped after sponge-cleaning Figure 2-1. Distribution of Percentage of Lead Found in Sponges, Wipes, and on Coupons (Wiped and Not Wiped), by Surface and Soil Types (Log-scale) 2-2 ------- to achieve for aqueous solutions, thus 30 dyne/cm was the lower limit of the range of surface tensions. Additionally, the effect of phosphate content on lead-cleaning efficacy was investigated by adding known amounts of anhydrous trisodium phosphate to the cleaning solutions corresponding to the amounts of 0,3,11, and 14 g phosphorus per gallon (g P/gal). The combination of these two factors provided 16 cleaning solutions to be tested. Laboratory staff prepared two types of surfaces—enamel- and latex-painted birch plywood—each one foot square (called coupons), and placed lead-containing synthetic soil on the surfaces. The lead-containing synthetic soil was a modification of ASTM D4488 soil, replacing the clay in the ASTM D4488 soil with NIST SRM 2710 (5,532 ug Pb/g), a contaminated soil from Montana. The two surfaces selected for contamination with the soil were intended to represent all common types of surfaces to be cleaned (e.g., walls, trim, kitchen cabinets). Two types of soil were used. One contained a small amount of vegetable oil to simulate dust contaminated with oils from cooking or human contact The other, a dry soil, contained no added oil. The lead loadings used in the study correspond to approximately 950 ug Pb/ft2 (dry soil on enamel-painted surfaces), 1,900 ug Pb/ft2 (dry soil on latex-painted surfaces), 850 ug Pb/ft2 (oily soil on enamel-painted surfaces), and 1,700 ug Pb/ft2 (oily soil on latex-painted surfaces). To obtain a reasonably even distribution of soil over the majority of the surface on latex-coated coupons, 4 mL of soil mixture was necessary. Only 2 mL of soil mixture was required to obtain the same coverage result on enamel-coated coupons. The coupons were soiled by a single technician according to a full factorial experimental design. A single technician then cleaned each coupon surface with a given cleaning solution using a sponge to remove the soil material and the associated lead. Half the coupons were then wiped using a baby wipe; the other half were not (The wipes used were pre-wetted, commercially available baby wipes containing purified water and propylene glycol, as per manufacturer's ingredients list, to wet the wipes and keep them wet for a long period of time.) All coupons were then cored. All sponge, wipe, and core samples were analyzed to measure the amount of lead in each type of sample. 2.2 Conclusions Based on the 128 sponge-cleaning tests, 64 wipe tests, 64 coupon tests from wiped surfaces, and 64 coupon tests from 64 non-wiped surfaces, the following conclusions were drawn. • Approximately 72 to 74 percent of the lead applied was removed by the sponge. • Approximately 1.3 to 1.6 percent of the lead applied was removed by the wipes after the surfaces were cleaned by the sponge. 2-3 ------- Approximately 20 to 23 percent of the lead applied remained on the coupons after sponge-cleaning and wiping. Approximately 22 to 26 percent of the lead applied remained on the coupons after sponge-cleaning only. • The total percentage of lead accounted for in this study was estimated at approximately 95 to 99 percent, leaving approximately 0.9 to 5.3 percent unaccounted for. The amount of lead picked up by the wipe from the sponge-cleaned surface was estimated at approximately 2 percent in the previous study. This estimate is comparable to the slightly lower estimate of 1.3 to 1.6 percent found in mis study. In contrast, the estimated amount of lead remaining on the cleaned surface, expressed in percentage of applied amount, is significantly higher in this study than in the previous study: 20 to 26 percent versus 7 percent. The estimate of 20 to 26 percent was directly estimated from cleaning tests in this study. Since neither sponges nor surface samples were analyzed in the previous study, the percentage of lead removed by a cleaner and sponge was based on a small set of wipe cleaning experiments. In that study, the assumption was made that two baby wipes would remove similar quantities of lead as would a cleaner and sponge. That estimate was found to be roughly 91 percent. By subtraction, the percentage of lead remaining on a cleaned and wiped surface was estimated at 100 percent - 91 percent - 2 percent = 7 percent. The analysis of the effect of surface tension and phosphate content on cleaning efficacy provided the following results: • Overall, surface tension and phosphate content had no statistically significant effect on the residual lead found on coupons. This is true whether the coupons were wiped or not after sponge cleaning. • When sponge and wipe results were examined, both surface tension and phosphate content had an overall statistically significant effect on cleaning efficacy. However, no consistent pattern in the effect of these two factors on cleaning efficacy could be found. That is, no monotonic relationship could be found between die levels (values) of these factors and the resulting cleaning efficacy. This lack of consistent pattern was found in sponges and wipes. For example: - Across all coupon surface types, soil types, and phosphate content levels, it was found that lower surface tension cleaning solutions are associated with better sponge cleaning. However, this significant surface tension effect is masked by interactions with the type of coupon surface and soil type. 2-4 ------- - When looking individually at the four combinations of surface type and soil type, surface tension was no longer predicting cleaning efficacy when using a sponge. Only when dry soil was applied to latex-painted surfaces did phosphate content affect cleaning efficacy when a sponge was used. However, no meaningful relationship between cleaning efficacy and phosphate content level could be found. In other words, cleaning efficacy did not increase or decrease consistently with phosphate content. - Surface tension had a small but significant effect on the ability of wipes to pick up lead from all surfaces. It was found that the percentage amount of lead picked up by the wipe increased with increasing surface tension of the cleaning solution. The effect of surface type and soil type on cleaning efficacy was also investigated. The analysis provided the following results: * Surface type (enamel- and latex-painted plywood surfaces), soil type (dry and oily), and their interaction had in most cases a significant effect on lead cleaning efficacy. • Although latex-painted surfaces are rougher than enamel-painted surfaces, the percentage of lead found in the sponge did not reflect that fact. However, wipes picked up a higher percentage lead from latex-painted surfaces than from enamel- painted surfaces after sponge-cleaning, possibly indicating that rougher surfaces are more difficult to clean. • The above finding could not be confirmed when looking at the residual lead on the coupons. In those cases (wiped and non-wiped coupons), the trend was counter-intuitive in that a higher residual lead was found on enamel- (smooth) than latex- (rough) painted surface. • Generally, an oily soil surface was more difficult to clean than a dry soil surface. 2.3 Recommendations Based on the above findings, no conclusive evidence was found to recommend trisodium phosphate (TSP) or high phosphate detergent cleaners for lead removal inside homes. In addition, the weak evidence found in the previous study that cleaners with lower surface tension appear to clean soiled surfaces slightly better than cleaners with high surface tension could neither be refuted nor strengthened. However, EPA still recommends that either a general all-purpose cleaner or a cleaner made specifically for lead should be used for both general cleaning and for post-intervention cleaning. Household cleaning 2-5 ------- using one of these cleaning agents is likely to remove more leaded soil and dust than does water alone. The extent to which these conclusions, based on laboratory investigation, apply to homes in real-life situations is a matter of judgment. Cleaning home interiors with a damp sponge or cloth will likely remove significant amounts of lead-containing soils. Water alone would do an adequate job, but considering that most cleaning is done by repeatedly wiping a soiled surface and rinsing the sponge or cloth into a bulk cleaning solution, a common household cleaner would probably help keep the soil in suspension, thus lessening the redeposition of the soil back onto the surface being cleaned. General home cleaning will thus further assist in the prevention of childhood lead poisoning. 2-6 ------- Section 3 Study Design This section provides the overall study design, including the selection of the cleaning agent, the tests performed, and the number of tests and their randomization. 3.1 Experimental Design The experimental design for this follow-up study was based on statistical results from the previous study. Most factors considered here are identical to those investigated in the previous study, with the exception of the number of cleaners and substrates. As before, baby wipes were used to wipe the coupons after they were cleaned with a sponge and the cleaning mixture. However, unlike in the previous study, the sponges, cleaning solutions, and rinse water were not discarded, but were analyzed for lead content. In addition, core samples of each coupon were taken, composited, and also analyzed for residual lead. It was further decided to perform two sets of tests as follows: • In one set of experiments, the coupons were soiled, then cleaned with the sponge plus cleaning solution plus water, and men wiped with baby wipes. • In the other set of experiments ("replicate" runs), the coupons were soiled, then cleaned with the sponge plus cleaning solution plus water. These coupons were not wiped with baby wipes so that the number of wipe lead analyses was reduced in an attempt to control cost and because the previous study already provided ample information on lead content of wipes. In summary, based on discussions among EPA and project staff, the previous lead- cleaning efficacy results, and the objectives of this follow-up study, the following design factors were considered in a full factorial experimental design: • A hand dishwashing detergent at 4 concentration levels corresponding to 4 surface tension values of approximately 30,40,60, and 70 dyne/cm • Anhydrous trisodium phosphate (TSP) concentration levels corresponding to approximately 0,3,11, and 14 grams of phosphorus per gallon (g P/gal) • 2 substrates: enamel on birch plywood and latex on birch plywood • 2 soils: oily and dry • Replication of tests 3-1 ------- This design layout resulted in a total of 4 surface tensions x 4 phosphate levels x 2 substrates x 2 soil types x 2 replications = 128 coupon tests. Under this scenario, two batches of soil mixture of each type of soil needed to be prepared because a single batch of soil mixture is sufficient for only 40 coupon tests, adding a blocking factor to the design and the sequence of tests. From this design, a test schedule was developed as follows. The first soil batch consisting of 8 oily mixtures and 8 dry mixtures was prepared (at the same time, as in the previous lead-cleaning study). Then half of the first set of tests (with wiping) and half of the second set of tests (without wiping) was completed. After these 64 coupon tests were completed, the second soil batch, again consisting of 8 oily mixtures and 8 dry mixtures, was prepared for the remaining coupon tests. Each cleaning solution was used on 4 coupons (4 combinations of 2 soil types and 2 substrates). All tests were performed on new coupons; that is, new birch plywood was painted with either latex (1 coat of primer and 1 top coat of paint) or enamel (2 top coats of paint) paint and cut into 12 in x 12 in coupons (the thickness of the dried paint film is unknown). The same procedures for coupon preparation, soil mixture preparation, soil mixture application, and coupon cleaning as were used in the previous study were followed. The procedures for preparing the cleaning solutions and coring the coupons are explained in Section 4.1. Samples were analyzed for lead according to the QAPjP for Pb-Cleaning Efficacy for Lead Abatement in Housing, Revision No. 4, July 12,1995.2 Additional protocols developed to address the modified digestion procedures of sponge and core samples can be found in Appendices B-l and B-2, respectively, of the above mentioned QAPjP.3'4 These appendices reflect the changes made to Appendix B in its terminology (sponge and core, respectively, instead of wipe) and in the volume of acid needed to digest the samples that were larger in weight than wipe samples. The test schedule based on this design is shown in Table A-l in Appendix A. The sequence of the cleaning solutions (combinations of surface tension and phosphate content) was randomized within soil batch, and the sequence for the coupon tests (soil and substrate) was randomized within cleaning solution. This design required the preparation of 32 cleaning solutions, each of a given surface tension (4 levels) and phosphate content (4 levels), in duplicate. A total of 128 coupons (32 cleaning solutions x 2 soil types x 2 substrates) were prepared, soiled, and cleaned. Of these 128 coupons, 64 were cleaned Table 3-1. Number of Cleaning Solutions Tested for Each Combination of Phosphate Content and Surface Tension Phosphate content (9 P/gal) 0 3 11 14 All 30 2 2 2 2 8 Surface tension (dyne/cm) 40 60 70 222 222 222 222 888 All 8 8 8 8 32 3-2 ------- with a sponge + cleaning solution + water. The remaining 64 coupons were cleaned with a sponge + cleaning solution + water and also wiped with baby wipes. The total number of cleaning solutions tested for each combination of phosphate content and surface tension in this design is shown in Table 3-1. 3.2 Cleaning Agent Selection A total of 32 commercially available cleaning agents, synthetic tap water of average hardness, and TSP were tested in the previous study. From the 32 cleaning agents, a single cleaner (a popular, commercial hand dishwashing detergent) was selected. The criteria for selection were that the cleaner be: • a phosphate-free cleaner, because TSP will be added to the cleaning solutions at various concentration levels. • a neutral to basic cleaner so as to avoid mixing an acidic cleaner with TSP (basic). • a cleaner that does not need to be used at full strength, such as out of a squirt bottle; such a cleaner would not allow the consumer to adjust concentration to change surface tension. • a cleaner that is easily measured out, that is, in a significant amount to be added to water (e.g., 1/2 gal). This criterion excluded laundry and dishwashing cleaners since they are used in small amounts in larger quantities of water. • a cleaner that is readily available hi households, such as a hand dishwashing cleaner. 3.3 Precleaning Tests To verify some of the results found in the previous study pertaining to the lead levels in the soil mixtures and the rod rinse,1 a small number of tests were performed without cleaning solution. Based on the above experimental design, verification tests, including soiling and wiping the coupons with two baby wipes each, were performed on a total of: • 2 soil mixtures x 2 batches of each soil mixtures x 2 substrates = 8 coupons Core samples of these coupons were also taken, although this step was not performed in the previous study. Samples were taken and analyzed by either ICP or GFAA for lead content as follows: 'The rod rinse is a mixture of a solvent and the soil left on the applicator rod after it was used to spread the soil on the coupon. See Section 4.1 for details of soil application procedure. 3-3 ------- 8 soil mixture samples (2 types of soil mixture x 2 batches of soil mixture each x 2 replications) 8 coupon core samples (4 enamel on birch and 4 latex on birch coupons) 8 rod-rinse samples (1 per coupon) 16 wipes (2 wipes per coupon) These eight precleaning tests were randomly inserted in the design layout shown in Table A-l in Appendix A as follows. Precleaning tests using a given soil batch (1 or 2) were performed when that soil batch was used for the coupon tests. In addition, the precleaning tests were always performed between two sets of tests using different cleaning solutions for ease of implementation. Except for these two restrictions, the placement of the precleaning tests was random within the sequence of the 128 coupon tests. Table 3-2 summarizes the combination and sequence of precleaning tests. Table 3-2. Test Schedule of Proposed Precleaning Tests Soil batch 1 1 1 1 2 2 2 2 Soil type Oily Oily Dry Dry Dry Dry Oily Oily Substrate Enamel Latex Latex Enamel Latex Enamel Enamel Latex Test sequence 1 2 3 4 5 6 7 8 3.4 Blank Soil Tests As was done in the previous study, a limited number of tests with "blank soil," that is, using soil without the leaded component, were performed to identify the magnitude and source of any contamination. A total of eight coupon tests, requiring the preparation of both oily and dry blank soil mixtures, were performed using cleaning solution Nos. 16 and 32 according to the test schedule shown in Table 3-3. Table 3-3. Test Schedule of Blank Soil Tests Soil type Oily Dry Dry Oily Dry Oily Dry Oily Phosphate level 0 0 0 0 11 11 11 11 Measurement method No wipe Wipe Wipe No wipe No wipe Wipe No wipe Wipe Substrate Enamel Enamel Latex Latex Latex Enamel Enamel Latex Surface tension 30 30 30 30 30 30 30 30 Cleaning solution 16 16 16 16 32 32 32 32 Test sequence 1 2 3 4 5678 3-4 ------- Samples were taken and analyzed for lead content by ICP followed by GFAA, if necessary, as follows: • 8 coupon core samples (4 enamel on birch, 4 latex on birch) • 8 sponge + cleaning solution + water (1 per coupon) • 4 wipe samples (1 per coupon, if wiped) Table 3-4 summarizes the number and types of field samples that resulted from this experimental design. Throughout this report, samples generated by the coupon preparation laboratory are referred to as field samples, hi contrast, samples generated in the analytical laboratory, such as method blanks, standard reference material samples, and laboratory control samples, are referred to as laboratory QC samples. A slight deviation from this classification is that matrix method blanks, such as blank wipes, blank sponges, and blank cores, although generated in the coupon preparation laboratory, are included with the laboratory QC samples. Table 3-4. Summary of Field Samples Generated Type of sample Soil mixture Rod rinse Coupon Sponge + cleaning solution + water Wipe All Precleaning tests 8 8 8 0 16 40 Blank soil tests 0 0 8 8 4 20 Cleaning tests 0 0 128 128 64 320 All 8 8 144 136 84 380 3-5 ------- Section 4 Laboratory Data Collection The cleaning tests were performed according to the experimental design described in Section 3.1 and the test sequence shown in Table A-l in Appendix A. Precleaning and blank soil tests were included as discussed in Sections 3.3 and 3.4. Both the preparation work for the coupons and the analytical lead work were performed by the same contractor as that reported in the previous lead-cleaning efficacy study. The following sections summarize the two types of data collection procedures, referred to as test data collection and quality control data collection procedures. 4.1 Test Data Collection A single technician implemented all laboratory procedures according to protocols. The protocols were those followed in the previous study and are included as part of the "Quality Assurance Project Plan for Pb-Cleaning Efficacy for Lead Abatement in Housing, Revision No. 4."2 Soil Mixture Preparation: Two types of soil were prepared following the same recipes as in the previous study: one soil mixture contained vegetable oil (oily soil), while the other mixture did not (dry soil). Each soil mixture consisted of 15 g of Standard Reference Material (SRM) 2710, a lead-containing soil with a concentration of 5,532 ug/g, as reported by MIST, 7.5 g of Norit A carbon black, 150 mL of mineral spirits, and 6.75 g of vegetable oil (oily soil only). Blank soils consisted of carbon black and mineral spirits, with the addition of vegetable oil for the oily blank soil. [Note: The boiling point of mineral spirits is 179° to 210°C; however, mineral spirits is a fairly volatile liquid. Mineral spirits was used in this study as a carrier to make the soil fluid so that it could be spread over the coupons. Vaporization of the mineral spirits was kept to a minimum by keeping the lid of the container tightly closed. A hole, just large enough to pass the pipette through it, was drilled through another lid. That lid was used while pipetting the soil mixture.] Cleaning Solution Preparation: The 16 unique cleaning solutions (4 phosphate levels and 4 surface tensions) required for the study were prepared in two batches each. The four target phosphate levels were achieved by adding anhydrous trisodium phosphate in amounts corresponding to concentrations of 0,3,11, and 14 g of phosphorus per 1 gal of cleaning solution. The phosphate content was calculated as phosphorus (P) contained in reagent grade anhydrous trisodium phosphate. The four surface tensions were obtained by adding approximately 0,0.008,0.050, and 6.36 g of the cleaning agent to 1 gal of synthetic hard water corresponding to the nominal surface tension levels of 70,60,40, and 30 dyne/cm, respectively. Once the cleaning solutions were prepared (i.e., after the 4-1 ------- addition of phosphate), their surface tension was measured twice per ASTM D1331, prior to cleaning the coupons. Coupon Preparation: A total of 152 coupons were prepared at the onset of the study. All coupons were made of birch plywood; half were painted with enamel paint and half with latex paint. (The painted material from which the coupons were made is referred to as the substrate.) Of the 152 coupons, 136 were soiled with leaded soil, including 128 test coupons plus 8 coupons for precleaning studies; 8 were soiled with blank soil (i.e., the soil contains no lead); and 8 were used as matrix method blanks (i.e., the coupons were analyzed as is). Soil Application: The leaded soil was spread over a coupon using an applicator rod, following the procedures described in the QAPjP.2 The applicator consisted of a 0.010-in diameter stainless steel wire wrapped around a 3/8-in diameter stainless steel rod. The rod was wrapped with wire over a 13-in length. A vee was produced between each wrap of the wire so that liquid would escape through the vee. A bead of liquid soil was spread across the coupon. The applicator rod was then repeatedly moved back and forth across the face of the substrate coupon to spread the liquid soil material as uniformly as possible over an area of approximately 10 x 10-in square. The rod was not allowed to roll on the substrate coupon surface to minimize the amount of soil retained on the applicator rod. The applicator rod was always parallel to the grain direction of the substrate coupon. Figure 4-1 provides a diagram of the soil application process. Coupon Cleaning: The soiled coupons were first cleaned using a new 3/4-in x 3-in x 6-in cellulose sponge to which the cleaning solution had been applied, according to the cleaning protocol. Following the cleaning with the sponge, the coupon was dried, then wiped with a single baby wipe according to the HUD Guidelines method. The sponge with its cleaning solution and water was kept for chemical analysis. Note that according to the study design, only half the coupons were wiped after cleaning. The wipes were also kept for chemical analysis. Coupon Coring: Coupon samples were taken for chemical analysis to quantify the amount of lead remaining on the surface of the coupon after cleaning and wiping. Nine core samples were taken from each coupon as shown in Figure 4-2. The core samples were generated by using a 1/2-in diameter wood-coring drill bit. The coring drill bit was designed to score the coupon at the circumference of the drill bit to reduce the generation of splinters outside the 1/2-in diameter core sample area. The coupon was scored first on both plane surfaces, then drilled through. After each drilling, the coring drill bit was brushed off to remove and collect adhering soil, paint, and plywood. The painted wood chips were collected and kept for chemical analysis. 4-2 ------- Applicator rod - stainless steel rod, spiral wrapped tightly with 0.010" stainless steel wire I "V" produced between each wrap of wire allows liquid to escape and spread fairly uniformly over coupon Coupon \ •Bead of liquid soil Rod is slid (not rolled) back and forth across bead of liquid soil to spread it over coupon Figure 4-1. Diagram of Soil Application Procedure 980276 4-3 ------- 12" 12" 980602 Figure 4-2. Diagram of Core Hole Locations on Coupon 4-4 ------- To estimate the average surface of the drilled cores, an estimate of the average diameter of the holes was obtained as follows. The diameter of three randomly selected holes in seven randomly selected coupons was measured. The 21 diameters ranged between 0.5095 in and 0.5250 in, with a mean of 0.5148 in and a standard deviation of 0.0051 in. Thus, the average surface of the 9 holes per coupon was calculated at 1.8736 in2, representing only a small fraction of the coupon surface. Furthermore, when soiling a coupon, the soil was applied to the entire 12-in coupon minus approximately a 3/4-in border. It is therefore assumed that the soiled surface is approximately 110.25 in2. However, since both sponging and wiping activities were performed over the entire surface of the coupon (i.e., 144 in ), it is assumed that the residual lead on the coupons is evenly spread over the entire surface. To obtain an estimate of the amount of lead remaining on the coupon (actually on the soiled surface of the coupon), the results from the composited nine core samples were adjusted upward to the soiled surface of the coupons. The final Pb result were thus expressed in total ug of Pb per coupon. The correction factor applied to the core sample Pb results was thus estimated at 76.86 (144/1.8736) and was applied to all core sample results in this study. Precleaning Tests: According to the study design, eight separate tests were performed to measure the quantity of lead applied to the coupons before cleaning (Section 3.3). For these precleaning tests, the leaded soil (oily and dry, one from each soil batch) was applied to the coupons (latex and enamel substrates) using the applicator rod according to the procedures used in all cleaner tests. The applicator rod was then rinsed and the rinsate, or rod-rinse sample, kept and analyzed for lead content. In addition, samples of the dry and oily soils were analyzed for lead content. The quantity of lead in the soil and that in the rod rifise provided an estimate of the quantity of lead applied before cleaning. The coupons soiled during these tests were wiped with two wipes and subsequently cored. No cleaner was used in these tests. Blank Soil Tests: Eight blank soil tests were performed using one cleaning solution from each batch and two coupons of each of two types. These tests are similar to the cleaner tests except that the soil applied to the coupons did not contain lead. These tests were performed to assess potential contamination during testing activities. Matrix Method Blanks: To assess potential lead contamination during the preparation steps of the coupons, a number of blank samples were collected: 7 blank sponges, 5 blank wipes, and 8 blank core samples. These samples were inserted into the analytical preparation batches and analyzed along with the test samples. Cleaner Phosphate Content and Surface Tension Measurements: The 32 cleaners, prepared in two sets, were obtained by mixing known amounts of the cleaning agent into a known amount of synthetic hard water to approximate the four surface tensions of 30,40, 60, and 70 dyne/cm specified in the experimental design. Synthetic hard water, chosen in consultation with EPA/OPPT, was prepared according to ASTM D4488. The average hardness across U.S. cities is near 150 ppm as calcium carbonate, the hardness of the 4-5 ------- prepared water. To each solution, anhydrous trisodium phosphate was then added as specified by the design to achieve the four phosphate content levels corresponding to 0,3, 11, and 14 g P/gal. Two surface tension measurements were taken from each of the 32 cleaning solutions (4 phosphate content x 4 surface tension x 2 batches), and then averaged. Phosphate content was calculated as grams of phosphorus/gallon, since reagent grade trisodium phosphate, anhydrous, was used as the phosphorus source. 4.2 Quality Control Data Collection All test samples (soils, rod rinses, sponges, wipes, and cores) were sent to the analytical laboratory for lead analysis. The test samples were digested in batches of 20 with additional quality control samples as required in the QAPjP and according to the Modified EPA Method 3050A used in this study. The wipe digestion method in the QAPjP required additional modifications to accommodate the sponge and core samples because they exceeded the 2-g sample weight limit of the method. Additional protocols were developed addressing the digestion of sponge and core samples and added to the QAPjP.3'4 An aliquot from each sample digest was analyzed for lead by inductively coupled plasma atomic emission spectroscopy (TCP) using modified EPA Method 6010A. Samples, which had a concentration less than ten times the ICP instrument detection limit, were analyzed using graphite furnace atomic absorption spectroscopy (GFAA) using a modified EPA Method 7421. A total of 1,321 lead analyses was performed for this study. Table 4-1 summarizes the number of samples of each type generated, separated by analytical method. 4-6 ------- Table 4-1. Type and Number of Samples by Analytical Method Sample type Test Samples Rod rinse Sponge Wipe Core Soil Matrix method blank (MMB) Total Percent (%) Analytical method ICP 8 136 86 144 8 21 403 64.3 GFAA 2 6 56 144 0 16 224 35.7 Total 10 142 142 288 8 37 627 100 Quality Control Samples Laboratory control sample (LCS) Method blank (MB) Standard reference material (SRM) Total Percent (%) Instrument QC samples Grand total Percent (%) 20 21 22 63 65.6 393 859 65.0 15 16 2 33 34.4 205 462 35.0 35 37 24 96 100 598 1,321 100 4-7 ------- Section 5 Quality Assurance/Quality Control An evaluation of the sample preparation and analysis results was performed throughout the course of the data collection by the Atomic Spectroscopy Facility Group Leader and by the program QA Officer (QAO). After final data reduction, an independent evaluation of the results was performed under the direction of the QAO. The final QC data were statistically analyzed by the project statistician. The results are presented in the following subsections. 5.1 Quality Assurance A complete systems audit was performed on this Work Assignment The system audit consisted of in-phase audits, facility audits, data audits, and a review and verification of the final report. The performance of the analytical system used for this Work Assignment was assessed using the results from the NIST SRM. The results of the performance assessment are discussed below in Section 5.2 under the Standard Reference Material topic. Sample identification and calculated lead amounts and recovery results are shown in Appendix B. These data pertain to all QC samples as well as all test samples generated during the project. The hard copy and computer records for the work performed by the contractor laboratory, including the tables for the final report, were audited. All sample identification codes and data were verified throughout the data handling process. The items verified during the audit are listed below. Accuracy and completeness for 15 data packets. • Completeness, compliance, and accuracy of the laboratory notebook pages, including the method of analysis, the project number, date of analysis, the analyst's name, the standards used for calibration, the steps performed in the preparation of the standards, and the dilutions. • Accuracy of the value used for NIST SRM 2710, based on the Certificate of Analysis information. • Accuracy of the sample identification codes in the report tables, using the sample preparation inventory listing from the test design. • Accuracy of the instrument responses presented as jig/mL for ICP and ng for GFAA in the data calculation tables, using the instrumental raw analysis data. 5-1 ------- • Accuracy of the initial calibration verification (ICV) control charts, using the percent recovery results from the data calculation tables, separately for ICP and GFAA. • Accuracy of the initial laboratory control sample (LCS) control charts, using the percent recovery results from the data calculation tables, separately for ICP and GFAA. • Accuracy of the SRM 2710 control charts, using the percent recovery results from the data calculation tables, separately for ICP and GFAA. All QC data were inspected in real time as they were collected and were reduced the following day. The problems found during this data audit were addressed in a letter to the EPA Work Assignment Manager and are discussed in the following section. 5.2 Quality Control This section presents the analysis of the lead levels found in the QC samples analyzed with the test samples. Three types of laboratory QC samples and one type of test QC samples were analyzed by ICP and GFAA according to the QAPjP.2 The QC samples included: • 21 method blank (MB) samples, used to demonstrate absence of laboratory and reagent contamination • 21 laboratory control samples (LCSs), used to monitor method performance and matrix effects • 22 standard reference material (SRM) NIST 2710 samples, used to measure the effectiveness of the digestion and analysis methods • 21 matrix method blank (MMB) samples, generated during the process of soiling and cleaning the coupons, to assess lead contamination during the coupon cleaning process and to determine background levels hi each matrix type: sponge, wipe, coupon, and liquid soil Method Blank (MB) Samples: In this study, two types of method blanks were prepared with each batch of samples: a method reagent blank (MB) and a matrix method blank (MMB). Both types of blanks are used to measure the extent of contamination problems associated with sampling, digestion, and analysis. The MB is used to measure the background levels of the reagents used for digestion plus any cross-contamination that might occur during the digestion procedure. The MMB is used to assess the background levels in the collection material, background levels in the reagents, and any cross- contamination that might occur during the digestion process. 5-2 ------- Twenty-one laboratory-generated MB samples were prepared with the test samples. Five of the 21-MB results are reported from ICP and the remaining 16 results are from GFAA. All of the MBs reported by ICP were less than three times the instrument detection limit. Four of the 16 GFAA MB samples had lead levels less than the detection limit (0.19 fig Pb/wipe or 0.06 ug Pb/core). Lead levels in the MB ranged from 0.06 to 26.8 //g. The MB result of 26.8 ug was considered an outlier after performing a Dixon Outlier test for the GFAA wipe MB results. Excluding the outlier, the average GFAA lead level found in the remaining 15 MBs analyzed by GFAA was 0.84 ug with a standard deviation of 0.92 ug. For a method blank to be acceptable for use with the accompanying samples, the concentration of the analyte of concern should not be higher than five percent of the measured concentration in the samples. In the wipe batch that contained an MB with an elevated lead background level, 8 of the 20 test samples prepared could be considered as having some background contamination. In this study, two types of method blanks (MB and MMB) were prepared with each batch of test samples to measure the extent of a contamination problem. The MMB is a more comprehensive measure of the background level than the MB because the MMB contains both reagents and matrix. The MMB prepared with this batch of wipes had a lead background less than detection limit and does not indicate significant lead background levels in the reagents, collection materials, or digestion procedure. Based on the background level for the MMB, the results for the test samples in this wipe batch should not be considered compromised. Laboratory Control Samples (LCSs): An LCS is a blank sample, spiked with a known amount of analyte being measured and digested along with the other samples in a batch. The LCS is used to monitor the method performance in the presence of a matrix. An LCS is prepared by spiking the analyte on a blank matrix being investigated. LCSs were prepared by spiking an MMB with 100 ug of lead (from a NIST-traceable solution) for a final digestion concentration of 1 ug/mL. Twenty-one LCSs (9 core, 6 sponge, 5 wipe, and 1 liquid soil) were analyzed, and the percent recoveries calculated. The results shown here use the GFAA recovery results from the core LCSs and ICP recovery results from the other three LCS matrices. One wipe LCS had a low recovery of 3.44 percent. This LCS was not spiked according to the procedure. This sample was determined to be an outlier using the Dixon's Outlier Test when compared with the wipe LCS results prepared and analyzed for this study. The poor performance for this LCS does not affect the results for the batch. In this program, two types of LCS samples were prepared and analyzed with each batch of samples, an aqueous spike and an SRM. The result for the SRM associated with this batch of wipe samples had a recovery of 102.6 percent. LCS percent recovery statistics are summarized in Figure 5-1 in the form of a QC chart and in Table 5-1. Excluding the outlier of 3.44 percent, two of the remaining results are below the lower control limit of 80 percent. 5-3 ------- Table 5-1. Laboratory Control Sample Results by Matrix Percent recovery Matrix (Instrument) Core (GFAA) Sponge (ICP) Wipe (ICP) Liquid soil (ICP) No. of samples 9 6 4a 1 Minimum 72.3 82.8 93.1 86.6 Maximum 99.0 100.1 101.4 — Mean 86.8 92.7 97.0 — Standard deviation 9.61 6.68 3.69 - • One outlier of 3.44 percent removed. The LCS acceptance criteria stated in the QAPjP2 are 80 percent to 120 percent recovery of Pb from the matrix. In this study, all of the LCS samples prepared with a sample matrix had acceptable recoveries and fell within the acceptance criteria for the LCS except for two core LCS samples. The core LCS samples had a lower mean value than the other matrices analyzed, which suggests that this matrix interferes with the recovery of Pb. The lowest value for the nine LCS samples prepared and analyzed was 72.3 percent. This recovery is within 1.5 times the standard deviation for this matrix type. When setting up control limits using the mean and the standard deviation for the core matrix, 72.3 percent recovery is in control, and all data should be accepted. Standard Reference Material (SRM) Samples: SRM samples were tested to monitor variations in the data from one analytical batch to another and to estimate method recovery for the analytical process. These tests were performed in an ongoing fashion in the laboratory and were not project specific. NIST SRM 2710 with a lead level of 5,532 ug Pb/g material was used to prepare the leaded soils in this study, and a 1-g aliquot of the same SRM was used in the preparation laboratory. Twenty-two SRM samples (8 core, 8 sponge, 5 wipe, and 1 liquid soil) were analyzed, and the resulting percent recovery calculated. SRM percent recovery statistics are summarized in Figure 5-2 in the form of a QC chart and in Table 5-2. Of the 22 recovery results, one wipe SRM at 78.7 percent was below the lower warning limit of 80 percent but above the lower control limit of 75 percent. 5-4 ------- Spiked LCS Recovery for Lead Using ICP TJA-61E or GFM Varian SpectrAA 300Z (Data are labeled by matrix type) 130% 120% - 110% - 100% - 90% 80% - 70% 4816-8B 4816-17 4816-13 4818-11 4816-23 4816-28 4818-20 4818-25 4818-26 4816-30 4816-37 4816-12 4816-8A 4816-5 4816-16 4816-24 4816-18 4816-21 4816-37 4816-30 4816-32 Reparation Batch Nurter hstrument% Recovery — LCL .. UCL -LWL . UAL Labels: W = Wipe; S = Sponge; C = Core; L = Liquid soil Figure 5-1. LCS Percent Recovery Control Chart 5-5 ------- IMST SRM 2710 Ftecovery for Lead Usirg ICPTJAr61E (Date are labeled by rralrbc type) 130% 120% 110% 100% 90% 80% 70% w c c I I I I I I II I I I I 481MB 4816-17 4816-13 4816-11 481643 481629 4816-345 4816-20 481625 481626 481631 4816-12 48164A 48164 4816-16 481624 481634a 4816-18 481621 481637 481630 481632 Reparation Batch Muter h6tnjTBrt% Recovery -. LCL .. ua . UAL Labels: W = Wipe; S = Sponge; C = Core; L = Liquid soil Figure 5-2. SRM Percent Recovery Control Chart 5-6 ------- Table 5-2. Standard Reference Material Results by Matrix Percent recovery Matrix Core Sponge Wipe Liquid soil No. of samples 8 8 5 1 Minimum 82.4 92.6 78.7 90.7 Maximum 95.4 103.9 106.9 - Mean 91.1 96.7 95.6 — Standard deviation 4.44 3.71 10.8 — All of the SRM results were within the acceptance criteria of the QAPjP. The data presented in Table 5-2 show that the results for all SRMs were within two standard deviations of the mean based on the matrix type. The good recoveries for the SRM suggest that the reported data for each matrix type is comparable to other batches of similar matrix that were digested and analyzed. Matrix Method Blank (MMB) Samples: Blank sponge, wipe, and core samples were used to determine the background levels, if any, in the materials used. One blank sponge, core, or wipe sample was included in each preparation batch according to matrix type. A total of 21 MMBs were analyzed by ICP (9 core, 7 sponge, and 5 wipe samples). Of the 21 MMBs, only five sponge batches are reported from ICP data in Table 5-3. The remaining 16 MMBs are taken from GFAA data because samples in the batch were less than 10 times the ICP instrument detection limit, necessitating analysis by GFAA. Two blank sponges showed high levels of lead: one at 25.1 ug Pb/sample (analyzed by GFAA), the other at 130.1 ug/sample (analyzed by ICP). These two high values were identified to be outliers using the Dixon's Outlier Test. None of the levels found in the MMBs were below the GFAA instrument detection limit. Statistics for the resulting lead levels are summarized in Table 5-3. Table 5-3. Matrix Method Blank Sample Results by Matrix Amount (ug) of lead per sample Matrix Core Sponge Wipe No. of samples 9 5' 5 Minimum 0.88 2.2b 0.34 Maximum 7.41 7.39° 2.47 Mean 3.52 4.02° 1.26 Standard deviation 2.34 1.90° 0.99 ' Two outliers of 25.1 ug and 130.1 ug were deleted. " Minimum value from GFAA analysis. c Values taken from ICP analysis. 5-7 ------- The MM8 provides a measure of the Pb background level in the matrix. Except for two sponge batches that showed significant lead levels in the MMB, the levels found in all other batches is insignificant. The acceptance criteria for the blanks require the blank concentration to be within three times the instrument detection limit. In all cases (except for the two sponge batches in question) the MMB met the acceptance criteria. Background levels in test samples are considered significant if the lead concentration of the test sample concentration is less than five times the MMB level (provided the MMB is greater than three times the instrument detection limit). Most of the samples prepared with the two MMBs in question had lead concentrations more than five times the MMB level. Four samples from each batch (8 samples total) could be considered as affected by the high lead levels in the MMBs. However, when analyzing the other quality control samples prepared with each batch, we consider the lead levels in the MMB to be isolated cases. The SRM, LCS, and MB in each of these two batches were within the acceptance limits of the QAPjP. If the contamination had been widespread, all other QC and test samples would have been affected. We conclude that the MMB, while significant, does not adversely affect the measurement for lead in the rest of the samples prepared in the respective batches. 5-8 ------- Section 6 Cleaning Solution and Soil Characterization The main objective of this study was to assess the effect of surface tension and phosphate content of the cleaning solutions on lead-cleaning efficacy. Sixteen cleaning solutions, each in two batches, were prepared to clean coupons previously soiled with leaded soil. The first step in assessing the effect on cleaning efficacy was to characterize the prepared cleaning solutions for phosphate content, surface tension, and the amount of lead deposited onto the coupons. 6.1 Cleaning Solution Characterization Based on the study design, 16 unique cleaning solutions were prepared using the selected cleaning agent at four concentrations to approximate the four surface tension levels of 30,40,60, and 70 dyne/cm. Anhydrous trisodium phosphate was added to these cleaning solutions in amounts corresponding to the four levels of 0,3,11, and 14 g P/gal of mixture. Two batches of each cleaning solution were prepared during the course of the coupon soiling, resulting in 32 cleaning solutions. The surface tension of each mixture was measured twice and their phosphate content was calculated. The measured characteristics are shown in Table 6-1. As shown in Table 6-1, the discrepancies between nominal and calculated phosphate content, expressed as g P/gal, are negligible. However, the differences between nominal and corrected measured surface tension levels are considerable. Figure 6-1 displays the differences (nominal minus measured) in the form of a boxplot. In all but one case, the measured level is below the nominal level. The differences are consistently the largest at the 60 dyne/cm level. Although, on the average, the differences are smaller at the 70 dyne/cm level (synthetic hard water without cleaning agent), the measurements at that level present the greatest variability. The surface tension values for the cleaning solutions without cleaning agent range from a low of 48.9 dyne/cm to a high of 71.2 dyne/cm, with an average of 60.8 dyne/cm and a standard deviation of 8.98 dyne/cm. In addition, the variations between soil batches are large, as shown by the pairs of measurements at each nominal surface tension level. These measured surface tension levels of the cleaning solutions were compared to those of the deionized water used to prepare the cleaning solutions. Twenty surface tension measurements were taken over a 3-month period; 19 of the measurements ranged from 66.6 dyne/cm to 71.0 dyne/cm (mean of 69.7 dyne/cm; standard deviation of 1.0 dyne/cm), with one outlying low value at 57.8 dyne/cm. Thus, the large variability in surface tension of the cleaning solutions containing no cleaning agent remains unexplained. 6-1 ------- Table 6-1. Phosphate Content and Surface Tension Statistics Soil batch 1 2 1 2 1 2 1 2 1 2 1 2 1 2 1 2 1 2 1 2 1 2 1 2 1 2 1 2 1 2 1 2 Phosphate content (g P/gal) Nominal level 0 0 0 0 0 0 0 0 3 3 3 3 3 3 3 3 11 11 11 11 11 11 11 11 14 14 14 14 14 14 14 14 Calculated 0 0 0 0 0 0 0 0 2.99 2.99 2.99 2.99 2.99 2.99 2.99 2.99 11.00 11.00 11.00 11.00 11.00 11.00 11.00 11.00 14.00 14.00 14.00 14.00 14.00 14.00 14.00 14.00 Weight of cleaning agent fa/gal) 6.29200 6.34000 0.04869 0.04898 0.00840 0.00847 0 0 6.33400 6.30200 0.04927 0.04978 0.00846 0.00829 0 0 6.36000 6.31000 0.04960 0.04935 0.00844 0.00833 0 0 6.33800 6.27400 0.04882 0.04894 0.00840 0.00836 0 0 Surface tension (dyne/cm) Nominal level 30 30 40 40 60 60 70 70 30 30 40 40 60 60 70 70 30 30 40 40 60 60 70 70 30 30 40 40 60 60 70 70 Corrected average* 24.5 24.9 34.5 38.1 47.5 50.4 66.8 71.2 28.3 28.8 33.8 37.8 57.0 48.0 67.8 53.3 27.8 27.9 35.2 36.4 45.8 44.7 68.1 49.9 28.1 25.6 32.8 31.6 43.7 47.7 60.1 48.9 Cleaning solution no. 16 25 9 21 8 27 3 17 2 28 5 23 1 29 10 30 7 32 12 18 14 31 13 26 11 24 4 19 15 22 6 20 Average of duplicate surface tension measurements. The measured surface tension corrected according to the ASTM test method for measuring surface tension. is 6-2 ------- 30 20 8 10 e £ -10 IL-- T7...- 20 30 40 50 60 70 80 Nominal surface tension (dyne/cm) Figure 6-1. Differences Between Nominal and Measured Surface Tension Levels 6-3 ------- The nominal surface tension levels were achieved by mixing a predetermined amount of the cleaning agent (see column 4 in Table 6-1) into synthetic hard water to which phos- phate was added as indicated above. (The nominal level of 6.36 g/gal was the level recommended by the cleaning agent manufacturer. The other two non-zero nominal levels of 0.008 and 0.050 g/gal were determined hi a range finding experiment prior to the cleaning tests.) The relationship between cleaning agent concentration and surface tension, across all phosphate levels, is shown in Figure 6-2. The concentrations are shown on a log scale. Note that the zero concentration results are artificially shown at the 0.0001 level (log scale) for comparison. As seen hi Table 6-1, increasing the surface tension from approximately 30 dyne/cm to 40 dyne/cm required a decrease in cleaning agent concentration from approximately 6.36 g/gal to 0.050 g/gal, requiring many dilutions of the cleaner. The average of the two surface tension measurements for each of the 32 cleaning solutions was analyzed in a two-way analysis of variance. The nominal surface tension and phosphate content and their interaction were included in the model. Neither phosphate content (p = 0.24) nor the interaction between surface tension and phosphate content (p = 0.59) were statistically significant. As expected, the nominal surface tension was highly significant (p < 0.0001). The least square mean differences between nominal and measured surface tensions (each with a standard error of 1.81 dyne/cm) were as follows: At 30 dyne/cm: 3.03 dyne/cm • At 40 dyne/cm: 4.96 dyne/cm At 60 dyne/cm: 11.9 dyne/cm • At 70 dyne/cm: 9.28 dyne/cm Based on these results, a decision was made to use the measured surface tension rather than the nominal surface tension levels in all subsequent statistical analyses. This means that surface tension will be treated as a covariate rather than a categorical variable in the analysis of variance modes. 6.2 Leaded Soil Characterization A number of precleaning samples were generated in the laboratory and then analyzed by ICP and GFAA, if necessary, to assess the amount of lead deposited onto the coupons by means of an applicator rod, the amount of lead cleaned off by the wipes, and that remaining on the coupons, without any cleaning process. A total of 40 soil, rod-rinse, wipe, and core samples were analyzed. SOIL SAMPLES: The dry and oily soil mixtures used in this study were prepared in two separate batches during the soiling process of the coupons. From each of these four batches, two samples, one of 2 mL and one of 4 mL, were taken and analyzed for lead 6-4 ------- 80 70 ?" «o j> § 1 " u i W 40 30 20 0.00 1 . 1 • i I I 1 i i i i i 001 0.0001 0.001 0.01 0.1 1 10 100 Amount of cleaning agant (g/gal) (log acale) Note: The actual 0 g/gal level of cleaning agent is represented on this graph as 0.0001 for plotting purposes only Figure 6-2. Relationship Between Cleaning Solution Concentration (Log Scale) and Surface Tension 6-5 ------- content The two amounts of 2 mL and 4 mL correspond to the amount of soil applied to plywood painted with enamel and plywood painted with latex, respectively. Thus, a total of eight soil samples were analyzed for lead content. None of these samples was analyzed by GFAA. ROD-RiNSE SAMPLES: Each soil sample was applied onto a coupon using a wire- wound rod. After each application, the rod was rinsed and the rinsate analyzed for lead. Thus, a total of eight rod-rinse samples were analyzed. Of these eight samples analyzed by ICP, two were reanalyzed by GFAA. WIPE SAMPLES: Each soiled coupon was wiped with two wipes, and each wipe was analyzed separately. Thus, a total of 16 wipes were analyzed by ICP. The eight first wipes were analyzed by ICP only, while three of the eight second wipes were reanalyzed by GFAA. CORE SAMPLES: Each coupon was cored as shown hi Figure 4-1. The nine core samples from each coupon were composited and analyzed by ICP for lead content, resulting in a total of eight core samples. Due to their low load levels, all eight core samples were reanalyzed by GFAA. The amount of lead found in the core samples was adjusted to reflect the ratio of core surface to coupon surface as explained in Section 4.1. The adjusted result is an estimate of the amount of lead found on the entire coupon. The precleaning lead results are summarized in Table 6-2. None of the lead amounts was below detection limit. For each of the 8 combinations of volume of soil mixture (2 mL, 4 mL), soil type (dry, oily), and soil batch (1,2), the fourth column in the table shows the total Pb amounts per sample measured in each of the 5 samples: soil, rod rinse, first wipe, second wipe, and coupon (core adjusted for total coupon surface). The next column shows these results in total Pb per unit of soil mixture (ug Pb/mL). These results are also shown in Figure 6-3 in the form of a boxplot. The last two columns of Table 6-2 show calculations toward Pb mass balance closure without use of a cleaner; that is, under ideal sampling and analysis conditions, the quantities of lead could be apportioned as follows: Pb in Soil - Pb in Rod rinse = Pb in Wipe #1 + Pb in Wipe #2 + Pb remaining on coupon For each combination of soil type and soil batch, the two quantities displayed in Column 6 are those for both sides of this equation. The last column in Table 6-2 shows the quantity of lead captured as a percentage of the lead applied onto each coupon. As shown in Table 6-2, the amount of Pb captured as a percent of the amount of Pb applied onto the coupon exceeds 100 percent for both dry and oily soils. An explanation of this result could lie in the fact that the amount of Pb remaining on a coupon was extrapolated based on the nine core samples taken from each coupon. These nine core samples represent on the average only 1.87 in2 or approximately 1.3 percent of the total coupon surface of 144 in2. It should be noted, however, that these figures are based on a small sample size (four dry soil tests and four oily soil tests). A more detailed lead mass balance analysis is presented in Section 7.6. 6-6 ------- Table 6-2. Precleanine Sample Lead Results Soil Soil type batch Sample type Pb amount (ug) Pb amount (ug/mL) Subtotal (ug/mL) Fraction* (%) 2 mL of soil mixture Dry 1 Soil Rod rinse Wipe No. 1 Wipe No. 2 Coupon 2 Soil Rod rinse Wipe No. 1 Wipe No. 2 Coupon Oily 1 Soil Rod rinse Wipe No. 1 Wipe No. 2 Coupon 2 Soil Rod rinse Wipe No. 1 Wipe No. 2 Coupon 974.70 33.68 759.86 21.12 319.73 964.72 26.26 831.31 93.74 209.06 783.50 19.65 641.24 14.43 274.39 909.29 19.03 764.21 34.47 260.55 487.35 16.84 379.93 10.56 1 59.86° 482.36 13.13 415.66 46.87 104.53 391.75 9.83 320.62 7.22 137.20 454.65 9.52 382.11 17.24 130.27 470.51" 550.35" 469.23 567.05 381.93 465.03 445.13 529.61 117 121 122 119 4 mL of soil mixture Dry 1 Soil Rod rinse Wipe No. 1 Wipe No. 2 Coupon 2 Soil Rod rinse Wipe No. 1 Wipe No. 2 Coupon Oily 1 Soil Rod rinse Wipe No. 1 Wipe No. 2 Coupon 2 Soil Rod rinse Wipe No. 1 Wipe No. 2 Coupon 1,931.40 61.33 1,399.90 63.50 496.51 2,004.60 42.34 1,480.10 136.65 379.68 1,550.10 52.83 1,119.60 124.99 442.70 1,987.00 70.21 1,549.10 126.30 416.57 482.85 15.33 349.98 15.88 124.13 501.15 10.59 370.03 34.16 94.92 387.53 13.21 279.90 31.25 110.67 496.75 17.55 387.28 31.58 104.14 467.52 489.98 490.57 499.11 374.32 421.82 479.20 522.99 105 102 113 109 Ratio of amount (d) over amount (b), in 100 percent. Amount = Soil amount minus rod-rinse amount. Core amount was adjusted for total surface of coupon. Amount = Wipe No. 1 + Wipe No. 2 + Core amounts. 6-7 ------- o> I * Oily coupon Oilywipe#2 Oily wipe#1 Oily rod Oily soil Dry coupon Drywipe#2 Drywipe#1 Dry rod Dry soil 1 1 m i — {Eh •ED- * 1 1 1 1 1 - H 1 \ \ \ H •n> '- 0- - i i i 100 200 300 400 Pb concentration 500 600 Figure 6-3. Distribution of Precleaning Lead Concentrations by Soil and Sample Types 6-8 ------- ANALYSIS OF SOIL LEAD CONCENTRATIONS: The two types of soil (dry and oily) were each prepared in two batches over the course of the laboratory study. The lead concentrations (ng of Pb on the coupon per milliliter of soil mixture used) obtained from the eight sets of precleaning samples were analyzed to estimate the average quantity of lead applied to the coupons and whether that quantity is affected by soil type and soil batch. Similarly to the previous study,1 the amount of Pb in the soil, adjusted for the volume of the soil mixture and then log-transformed, was analyzed by analysis of variance (ANOVA). The two factors, soil batch and soil type, and their interaction, were included in the model. Both factors and their interaction were significant at the 5 percent significance level: soil batch (p = 0.0122), soil type (p = 0.0066), and interaction (p = 0.0191), based on a total of 8 samples. The least-square geometric mean concentrations and their 95 percent confidence intervals are as follows: Dry soil: 488.4 (465.5 to 512.3) ug Pb/mL of soil mixture Oily soil: 430.3 (410.2 to 451.4) ug Pb/mL of soil mixture The result was an average ratio of the lead concentration in the dry to oily soil mixture of 1.13. These lead levels are slightly different from those found in the previous study (dry soil at 464.0 ug/mL; oily soil at 440.2 ug/mL), and their ratio exceeds the ratio of 1.04 determined from the recipes for the two soil mixtures. The larger confidence intervals as compared to those from the previous study are mainly due to the smaller sample size (8 versus 48). ANALYSIS OF ROD RINSE LEAD CONCENTRATIONS: The amount of lead that remained on the applicator rod after applying the soil mixture to the coupons was analyzed in a similar fashion to that of soil samples. The effect of soil batch and soil type on the log- transformed lead concentration in the eight rod-rinse samples was estimated by ANOVA. Neither factor—soil batch (p = 0.64), soil type (p = 0.52)—nor their interaction (p = 0.29) had a significant effect on the log-transformed lead concentration. The least-square geometric mean concentrations and their 95 percent confidence intervals are as follows: Dry soil: 13.8 (9.7 to 19.6) ug Pb/mL of soil mixture Oily soil: 12.1 (8.5 to 17.3) ug Pb/mL of soil mixture These levels represent approximately 2.8 percent of the amount of lead in the soil (either dry or oily). ANALYSIS OF SOIL MINUS ROD-RINSE LEAD CONCENTRATIONS: The difference between the amount of lead in each soil sample and that in the corresponding rod-rinse sample was used to estimate the amount of lead applied to the coupons. Again, the log- transformed differences, adjusted for the volume of each soil mixture, were analyzed by ANOVA using the same two factors and their interaction as above. Both factors and their interaction were significant at the 5 percent significance level: soil batch (p = 0.0074), soil type (p = 0.0046), and interaction (p = 0.0161), based on a total of 8 samples. The least- 6-9 ------- square geometric mean concentrations and their 95 percent confidence intervals are as follows: Dry soil in soil batch No. 1: 469.0 (441.0 to 498.8) ug Pb/mL of soil mixture Dry soil in soil batch No. 2: 479.8 (451.1 to 510.2) ng Pb/mL of soil mixture Oily soil in soil batch No. 1: 378.1 (355.5 to 402.1) ug Pb/mL of soil mixture Oily soil in soil batch No. 2:461.9 (434.3 to 491.2) ng Pb/mL of soil mixture Due to the highly significant interaction between soil type and soil batch (see the large difference between oily batch Nos. 1 and 2 soils), all lead amounts quantified in the sponge, wipe, and core samples were adjusted for the above soil lead levels separately for each soil type and soil batch when estimating cleaning efficacy (Section 7). 6-10 ------- Section 7 Statistical Results This section presents the statistical analysis results as they relate to the study objectives: (1) determine the lead-removal efficacy of a cleaning solution as a function of its surface tension and phosphate content; (2) quantify the amount of lead actually removed from the coupon surface by the sponge-cleaning procedure; and (3) quantify the amount of lead remaining on the surface of the test coupon. In accordance with the study design, lead data were obtained from cleaning tests performed on 128 coupons. All coupons were cleaned using a sponge and a cleaning solution. Half of the coupons were then wiped with a baby wipe; the other half were not wiped; all coupons were cored. The statistical analysis results of the amount of lead in each of the four sample types—sponge, wipe, coupon with wiping, coupon without wiping—are presented separately in the following sections. The effect of surface tension and phosphate content of the cleaning solution on the results is discussed in each section. 7.1 Treatment of Surface Tension in the Statistical Analyses According to the full factorial experimental design presented in Section 3.1, all combinations of phosphate content (0,3,11, and 14 g P/gal), surface tension (30,40,60, and 70 dyne/cm), soil type (dry and oily), soil batch (1 and 2), and substrate (enamel- and latex-painted plywood) were tested twice. This replication was, in effect, a pseudo- replication, since the testing required that the 16 cleaning solutions (4 phosphate levels x 4 surface tension levels) be prepared in two batches, resulting in 16 pairs of cleaning solutions. The two theoretically identical cleaning solutions in each pair, however, were each characterized as to their surface tension and phosphate content. As was shown in Table 6-1, the discrepancies between pairs of surface tension measurements are consider- able at the higher nominal surface tension levels (60 and 70 dyne/cm), while the discrep- ancies between measured and nominal phosphate levels are negligible. Therefore, it was decided that the characterization of the cleaning solution in its ability to wet a surface would be more reliably characterized in this study by using the measured surface tension of each cleaning solution. Thus, in all subsequent statistical analyses, the measured surface tension, rather than the four nominal levels, was used as a predictor variable for lead- cleaning efficacy of the cleaners. Surface tension was treated as a continuous independent variable, or covariate, in the statistical analysis. 7.2 Percentage Amount of Lead Removed by Sponge For each cleaner test, the amount of lead applied to the coupon was predicted by the amount of lead in the soil minus the amount of lead in the rod rinse (Section 6.2). The estimates of lead quantities applied, separately for each batch of dry and oily soil, were 7-1 ------- 469.0 ug/mL for dry soil from batch 1; 479.8 ug/mL for dry soil from batch 2; 378.1 ug/mL for oily soil from batch 1; and 461.9 ug/mL for oily soil from batch 2. The dependent (response) variable used in the analysis was the amount of lead removed by the sponge expressed as a percentage of the quantity of lead applied on the coupon. The quantities of lead applied, expressed in ug/mL of soil mixture, were adjusted for the amount of soil mixture applied, that is, 2 mL on enamel-painted coupons, and 4 mL on latex-painted coupons. The dependent variable was further log-transformed for statistical analysis; thus, the quantity, ln[(amount Pb removed by sponge/amount Pb applied) x 100] is the variable analyzed. An analysis of covariance of the log-transformed percentage of lead removed by the sponge was performed. The main effects (phosphate content, soil type, and substrate) and all their two- and three-way interactions were included in the model. Soil batch was included as a blocking factor. Surface tension was treated as a continuous variable, or covariate, and was crossed with all other terms included in the model. Thus, a total of 13 terms were included in the model. A significance level of 5 percent was selected throughout. The data were inspected for statistical outliers, based on the extreme studentized residuals. A total of six outliers were sequentially excluded from analysis (e.g., one at a time, and the model rerun each time). Additionally, based on the significance level (p-value) of the F-statistic calculated for all terms in the model, terms in the model were sequentially removed from analysis if the F-value was below 1.5. This is based on the assumption that although a factor or interaction might not be statistically significant (i.e., p < 0.05), the inclusion of that factor if its F-value is above 1.5 will provide a more sensitive test for the remaining statistically significant terms in the analysis of variance. The final results from this analysis of covariance are summarized in Table 7-1. All main effects and interactions with an F-value of 1.5 or more are included in the model. Only those main effects and interactions with a p-value of 0.05 or more are considered to be statistically significant. Overall, the geometric mean percent amount of lead removed by the sponge is estimated at 72.7 percent, with a 95 percent confidence interval of 71.5 to 73.9 percent. Of the main effects and interactions included in Table 7-1 (all with F-values above 1.5), only three are statistically significant at the 5 percent level: the three-way surface tension by substrate by soil type interaction (p = 0.0006); the covariate, surface tension (p = 0.0015); and the two-way surface tension by phosphate content interaction (p = 0.0210). Note that phosphate content is not a significant factor in this model. 7-2 ------- Table 7-1. Analysis of Covariance Results: Cleaning Efficacy of Sponges Dependent (response) vgriable Number of observations Root mean square error Mean response Factor Surface tension Phosphate Substrate Soil type Surface tension * phosphate Phosphate * substrate Surface tension * substrate * soil type Log-transformed percentage of lead removed using sponge to clean coupons 122 (6 statistical outliers removed) 0.0907 (corresponding to a coefficient of variation in the untransformed unit of 9.5 percent) 4.2859 (corresponding to a geometric mean in the untransformed unit of 72.7 percent) Degrees of freedom 1 3 1 1 3 3 3 Sum of squares 0.0871 0.0410 0.0201 0.0153 0.0835 0.0557 0.1537 Mean square 0.0871 0.0137 0.0201 0.0153 0.0278 0.0186 0.0512 F ratio 10.59 1.66 2.44 1.86 3.38 2.25 6.23 Prob>F 0.0015 0.1801 0.1210 0.1751 0.0210 0.0863 0.0006 Whole-model analysis of variance test Source Model Error Corrected total Degrees of freedom 15 106 121 Sum of squares 0.7448 0.8722 1.6170 Mean square 0.0497 0.0082 F-ratio 6.03 Prob>F 0.0001 In this overall covariance model, surface tension has a statistically significant slope of -0.0036 ln(percentage amount of lead removed) per dyne/cm [with a standard error of 0.0017 ln(%) per dyne/cm]. The negative overall slope would indicate that the percentage of lead removed by the sponge decreases with increasing surface tension, or conversely, that lower surface tension cleaning solutions are associated with better sponge cleaning. However, the significant three-way interaction between surface tension (covariate) and the two-way interaction of substrate by soil type indicates that the regression lines of percentage lead removed by the sponge versus surface tension in the four cells defined by substrate type (enamel and latex) and soil type (dry and oily) are not parallel. The analysis of covariance was therefore followed up by four separate analyses of covariance, one for each of the four combinations of substrate and soil type. Phosphate content was included as a main effect, along with surface tension (the covariate), and then* interaction. The inter- action term, surface tension by phosphate content, was not significant in any of the four models. Thus, the four analysis of covariance models were rerun without that term, including the covariate and the main effect only. The data were checked for statistical outliers and two additional outliers were removed. Following sequential removal of non-significant effects (F-value below 1.5), only one model was significant: phosphate content was statistically significant (p = 0.0005) for the 7-3 ------- latex and dry soil combination. Surface tension was not significant in any of the models. Table 7-2 summarizes the percentage of lead removed by the sponge as a function of phosphate content when cleaning latex-painted coupons soiled with dry soil. These statistics include the least-square geometric mean percent amount of lead removed by the sponge and its 95 confidence limits. These statistics are also displayed in Figure 7-1 and show an inconsistent trend across the four levels of phosphate content. The largest percentage of lead (78 percent) is removed when the phosphate content of the cleaning solution is 3 g P/gal, then decreases with increasing phosphate content; the lowest cleaning efficacy (67 percent) is obtained when the cleaning solution contains no phosphate. Table 7-2. Mean Cleaning Efficacy of Sponges by Phosphate Content When Used on Latex-Painted Coupons Soiled with Dry Soil Phosphate content (9 P/gal) 0 3 11 14 Percentage of Pb removed by sponge (%) Mean 67 78 70 69 95% Confidence limits Lower 63 74 66 65 Upper 70 83 74 73 85% Phosphate content (g P/gal) ••-Mean 95% LL 05% UL Figure 7-1. Mean Cleaning Efficacy of Sponges versus Phosphate Content When Used on Latex-Painted Coupons Soiled with Dry Soil 7-4 ------- The percent of lead removed by the sponge could not be predicted by the surface tension of the cleaning solution for the four combinations of substrate and soil type. Nevertheless, for illustrative purposes, Figure 7-2 shows a scatterplot of the percentage amount of lead removed by the sponge as a function of surface tension, separately for each combination of substrate and soil type. In each case, a regression line on the log-scale is shown, although not significant. Regression statistics are summarized in Table 7-3, showing the slope (on the log-scale) and intercept of each regression, noting that neither regression is significant. Table 7-3. Regression Statistics of Percent Lead Removed by Sponge versus Surface Tension (Nonsignificant Results) Substrate type Enamel Latex Soil type Dry Oily Dry Oily No. of measurements 29 31 32 28 Intercept* (%) 77 84 72 71 Slope of surface tension" -0.0013 -0.0013 -0.0004 -0.0007 Significance level (p-value) 0.29 0.25 0.72 0.59 " Intercept in untransformed scale. b Slope on log-scale. In summary, except for the single case of latex-painted coupons soiled with dry soil in which phosphate content was statistically significant, none of the factors considered in the models—surface tension and phosphate content—had a significant effect on the amount of lead removed by the sponge, expressed as a percent of lead applied. 7.3 Percentage Amount of Lead Removed by Wipe Of the 128 coupons soiled and cleaned using the sponge and the cleaning solution, half were wiped with a baby wipe. The design used was a balanced full factorial design with respect to phosphate content, nominal surface tension, substrate, and soil type. How- ever, soil batch was confounded with the cleaning solutions as per design (Appendix A) and was not included in the analysis. The statistical approach for analysis of the cleaning efficacy of the wipes was similar to that above, with the omission of soil batch. The log- transformed percentage amount of lead removed by the wipe was analyzed in an analysis of covariance, including all factors, their two-way interactions, and selected three-way interactions. Terms in the models for which the F-value was below l.S were excluded from the model in a sequential fashion. The final analysis of covariance model results are shown in Table 7-4. 7-5 ------- Enamel, Dry Soil f Enamel, Oily Soil £4.4 I 4.3 £4'2 *4, o o o 00 g4gl—I—I—I—I—I—I S 20 30 40 50 60 70 80 Surface tension (dyne/cm) Latex, Dry Soil JL I4'5 « £4.4 •p §4.3 £ 2,4.2 a. • 41 I ' 11111 o ft o ° o 0 0 -oO°° 0 „ ° 0 ° 0 0 . °0 0 1 1 1 1 1 20 30 40 50 60 70 80 Surface tension (dyne/cm) 20 30 40 50 60 70 80 Surface tension (dyne/cm) Latex, Oily Soil i4.2- i4.1 4.Q o o - o o '20 30 40 50 60 70 80 Surface tension (dyne/cm) Figure 7-2. Percent Lead Removed by Sponge Versus Surface Tension, Separately by Substrate and Soil Types 7-6 ------- Table 7-4. Analysis of Covariance Results: Cleaning Efficacy of Wipes Dependent (response) variable Number of observations Root mean square error Mean response Factor Phosphate Substrate Soil type Surface tension Phosphate * substrate Phosphate * substrate * soil type Log-transformed percentage of lead removed using baby wipes to clean coupons 64 0.4253 (corresponding to a coefficient of variation in the untransformed unit of 53 percent) 0.3879 (corresponding to a geometric mean in the untransformed unit of 1.47 percent) Degrees of freedom 3 1 1 1 3 7 Sum of squares 4.70 9.68 7.14 2.00 3.19 2.60 Mean square 1.57 9.68 7.14 2.00 1.06 0.37 F ratio 8.66 53.51 39.47 11.04 5.87 2.05 Prob>F 0.0001 0.0001 0.0001 0.0017 0.0017 0.0676 Whole-model analysis of variance test Source Model Error Corrected total Degrees of freedom 16 47 63 Sum of squares 30.39 8.50 38.89 Mean square 1.90 0.18 F-ratio 10.50 Prob>F 0.0001 The geometric mean percentage amount of lead removed by wipes is estimated at 1.47 percent, with a 95 percent confidence interval of 1.32 to 1.64 percent. As seen in Table 7-4, substrate and soil type account for a large proportion of the variance in the data explained by the model. Except for the marginally significant three-way interaction (phosphate content by substrate by soil type, with a p-value of 0.0676), all the effects shown in Table 7-4 are highly significant. Surface tension has an overall significant slope of 0.0141 ln(percentage amount of lead removed) per dyne/cm [with a standard error of 0.0042 ln(%) per dyne/cm]. The positive slope indicates that the percentage of lead removed by the wipe increases with increasing surface tension, possibly indicating that a larger percentage of lead amount remained on the coupon surface following sponge cleaning when using a cleaning solution with higher surface tension. This finding is in agreement with that found earlier where, overall, the sponge cleaning efficacy increased with decreasing surface tension of the cleaning solution (Section 7.2). It should be noted that, although highly significant (p-value < 0.0001), the slope of 0.0141 ln(%) per dyne/cm is small, especially when considering the available range of surface tension of 30 to 70 dyne/cm. Separately for each level of phosphate content, substrate type, and soil type, Table 7-5 shows the geometric mean (and 95 percent confidence limits) percentage of lead removed 7-7 ------- by the wipe. The results for phosphate content are also presented in Figure 7-3, showing a lack of consistent pattern across the levels of phosphate content. The results in Table 7-5 also show that a higher percentage of lead amount is removed by the wipe from latex- painted surfaces than from enamel-painted surfaces, and when using oily soil rather than dry soil. This finding would suggest that latex-painted surfaces (rougher than enamel- painted surfaces) and oily soils are more difficult to clean. In summary, the mean per- centages of amount of lead removed by the wipe were overall in the range of 1.00 percent to 2.24 percent, so all were relatively small and of little practical importance. Table 7-5. Mean Cleaning Efficacy of Wipes, Separately for Phosphate Content, Substrate Type, and Soil Types Factor Phosphate content (9 P/gal) Substrate Soil type Factor 0 3 11 14 Enamel Latex Dry Oify Percentage of Pb removed by wipe (%) Mean 2.24 1.52 1.05 1.32 1.00 2.17 1.06 2.06 95% Confidence limits Lower 1.79 1.21 0.84 1.05 0.86 1.87 0.91 1.77 Upper 2.81 1.90 1.32 1.65 1.16 2.53 1.23 2.40 Phoiphit* content (g P/gil) |.»M««n 95% It A »»* UL Figure 7-3. Mean Cleaning Efficacy of Wipes Versus Phosphate Content 7-8 ------- For completeness and comparison to Section 7.2, the percentages of amount of lead removed by wipes (on log-scale) are plotted versus surface tension in Figure 7-4, separately for the four combinations of substrate and soil type. 7.4 Residual Lead Remaining on Coupon After Sponge- Cleaning and Wiping Half the coupons were cleaned with a sponge and then a wipe. The results from these 64 coupons were used in this analysis. The same design factors as those used in the analysis of covariance of wipe results apply here. The dependent (response) variable used is as before the log-transformed percentage of lead remaining on the coupon. Again, the denominator of the fraction is the amount of lead applied to the coupon before any cleaning activity, not that remaining on the coupon after cleaning. Table 7-6 summarizes the analysis of variance results. Of all the main effects included in the model—phosphate content, surface tension (covariate), soil type, and substrate—and their two- and three-way interactions, only the main effects for substrate and soil type remained in the model after excluding all terms with an F-value below 1.5. In summary, the geometric mean percentage amount of lead remaining on the coupons was 21.5 percent, with a 95 percent confidence interval of 19.9 to 23.3 percent. Neither surface tension nor phosphate content affected the residual lead remaining on coupons after sponge-cleaning and wiping. Table 7-7 shows the geometric mean residual lead remaining on the coupons, separately for substrate and soil type. Based on this analysis, more lead remained on enamel-painted plywood (25 percent) than on latex-painted plywood (19 percent), which contradicts the notion that a smooth surface is more easily cleaned than a rough surface. Also, residual lead is higher on surfaces soiled with oily soil (24 percent) than on surfaces soiled with dry soil (20 percent); this seems intuitive, since oily soil adheres more easily to the surface and is thus more difficult to remove. Again, for completeness and comparison to the previous results, the percentages of amount of lead remaining on the coupons after sponge cleaning and wiping (on log-scale) are plotted versus surface tension in Figure 7-5, separately for the four combinations of substrate and soil type. 7.5 Residual Lead Remaining on Coupon After Sponge- Cleaning Only Sixty-four coupon results from the coupons that were only sponge-cleaned were analyzed to assess the effect of the design factors on the residual lead remaining on the coupons. The same approach as in Section 7.4 was followed. The analysis of covariance model first included all main effects—phosphate content, surface tension (covariate), soil 7-9 ------- Enamel.Dry Enamel.Oily JO a. -1 -2 20 30 40 50 60 70 Surface tension (dyne/cm) Latex.Dry e £i O- •s -1 -2 S. 20 30 40 50 60 70 Surface tension (dyne/cm) Latex.Oily I1 O- "5 -1 5 -2 £ 20 30 40 50 60 70 Surface tension (dyne/cm) JO a. •5 -1 -2 20 30 40 50 60 70 Surface tension (dyne/cm) Figure 7-4. Mean Cleaning Efficacy of Wipes Versus Surface Tension, Separately by Substrate and Soil Types 7-10 ------- Table 7-6. Analysis of Variance Results: Residual Lead on Coupons After Cleaning with Sponge and Wipe Dependent (response) variable Number of observations Root mean square error Mean response Factor Substrate Soil type Log-transformed percentage lead remaining on coupons after sponge-cleaning and wiping 62 (2 statistical outliers removed) 0.3079 (corresponding to a coefficient of variation in the untransformed unit of 36 percent) 3.0682 (corresponding to a geometric mean in the untransformed unit of 21 .5 percent) Degrees of freedom 1 1 Sum of squares • 1.08 0.47 Mean square 1.08 0.47 F ratio 11.37 4.98 Prob>F 0.0013 0.0294 Whole-model analysis of variance test Source Model Error Corrected total Degrees of freedom 2 59 61 Sum of squares 1.55 5.59 7.14 Mean square 0.78 0.09 F-ratio 8.18 Prob>F 0.0007 Table 7-7. Residual Lead on Coupons After Cleaning with Sponge and Wipe by Substrate and Soil Type Substrate Enamel Latex Soil type OHy Percentage of Pb remaining on coupon (%) Mean 25 19 20 24 95% Confidence limits Lower 22 17 18 21 Upper 28 21 22 26 7-11 ------- Enamel, Dry Soil Enamel, Oily Soil I 4.U 3.5 3.0 2.5 'o ' ' ' " * ° 0 0 B 2 —^ o o o o 0 1 1 1 1 jj-4.0 € f 3.5 1 |3.0 ij. ^ 12.5 £ 1 M 20 30 40 50 60 70 $ *'2 I 1 1 1 0 ° ° ° ° - _ o 0 o V • 1 1 1 1 0 30 40 50 60 7 Surface tension (dyne/cm) Latex, Dry Soil '4.0 f3.5h §>3.G I | 2.5; £ 2*0 30 40 50 60 70 Surface tension (dyne/cm) Surface tension (dyne/cm) Latex, Oily Soil € 3.5 1 m O f\ 73.C w 12.5 £ §on o o ° 0 °o ° o % 0 o oo • •• 1 1 1 1 Surface tension (dyne/cm) Figure 7-5. Residual Lead Remaining on Coupons After Sponge Cleaning and Wiping Versus Surface Tension, Separately by Substrate and Soil Types 7-12 ------- type, and substrate— and their two- and three-way interactions. Those terms with F-values below 1.5 were excluded sequentially from the model. Table 7-8 summarizes the final analysis of covariance results. One main effect, substrate, and a large number of interactions remained in the model; however, most were not statistically significant at the 5 percent significance level but were retained in the model to improve the sensitivity of the F-test for the other terms in the model. Overall, the geometric mean residual lead remaining on the coupons after sponge-cleaning only was 24.2 percent, with a 95 percent confidence interval of 22.2 to 26.4 percent. This percentage is slightly above that obtained for sponged and wiped coupons (21.5 percent). Table 7-8. Analysis of Covariance Results: Residual Lead on Coupons After Cleaning with Sponge Only Dependent (response) variable Number of observations Root mean square error Mean response Factor Substrate Surface tension * phosphate content Surface tension " substrate Phosphate content * soil type Substrate * soil type Phosphate * substrate * soil type Log-transformed percentage lead remaining on coupons after cleaning with sponge only 64 0.3408 (corresponding to a coefficient of variation in the untransformed unit of 41 percent) 3.1880 (corresponding to a geometric mean in the untransformed unit of 24.2 percent) Degrees of freedom 1 3 1 6 1 6 Sum of squares 0.53 0.55 0.28 1.10 0.37 1.31 Mean square 0.53 0.18 0.28 0.18 0.37 0.22 F ratio 4.60 1.59 2.41 1.58 3.22 1.88 Prob>F 0.0378 0.2067 0.1280 0.1754 0.0799 0.1071 Whole-model analysis of variance test Source Model Error Corrected total Degrees of freedom 20 43 63 Sum of squares 7.22 4.99 12.21 Mean square 0.36 0.12 F-ratio 3.11 Prob>F 0.0009 7-13 ------- As shown in Table 7-8, substrate (enamel- or latex-painted plywood) is the only significant effect in this model (p = 0.0378). The two interactions, substrate by soil type (p = 0.0799) and phosphate by substrate by soil type (p = 0.1071), are only marginally significant. Table 7-9 summarizes the geometric mean percentage amount of lead remaining on the coupons and its 95 percent confidence limits for the two types of substrates. As for coupons that were sponged and wiped, a large percentage amount of lead remains on enamel-painted surfaces (26 percent) than on latex-painted surfaces (22 percent). Again, this is counter-intuitive since enamel-painted surfaces are smoother and therefore would be easier to clean. Table 7-9. Residual Lead on Coupons After Cleaning with Sponge Only by Substrate Substrate Enamel Latex Soil type Percentage of Pb remaining on coupon (%) Mean 26 22 95% Confidence limits Lower 23 19 Upper 30 25 Neither phosphate content nor surface tension are significant predictors of residual lead on coupons after sponge cleaning only. For completeness, residual amounts of lead (on log-scale) were plotted versus surface tension, separately for the four combinations of substrate and soil type. The plots are shown in Figure 7-6. 7.6 Estimation of Lead Mass Balance In contrast to the previous study,1 lead results in this study were available for all the components in the soiling and cleaning steps. That is, the amount of soil applied to the coupon was estimated, as was that picked up by the sponge and that by the wipe (if a wipe was used), and that remaining on the coupon. Thus, for each individual coupon, the total amount of lead accounted for can be estimated by simply adding up the various components (sponge plus wipe plus coupon or sponge plus coupon). The percentage of total lead accounted for in each cleaning test was calculated and then analyzed in the same fashion as were previous response variables. An analysis of covariance of the log- transformed total percentage lead was performed using all the factors—phosphate content, surface tension (covariate), soil type, soil batch, and substrate—and their two- and three- way interactions in the statistical model. Again, terms with an F-value below 1.5 were excluded in a sequential fashion. The analysis of co variance results are presented in Table 7-10. 7-14 ------- Enamel, Dry Soil Enamel, Oily Soil • i 14 I I |3 1 B a h 11111 - o 0 0 0 n oa o 0 0 „ - O O ° 0 SJ * * f * 30 40 50 60 70 8 s I' £ Surface tension (dyne/cm) Latex, Dry Soil 30 40 SO 60 70 80 Surface tension (dyne/cm) f4 I £ I I £ 30 40 50 60 70 80 Surface tension (dyne/cm) Latex, Oily Soil \0 30 40 SO 60 70 80 Surface tension (dyne/cm) Figure 7-6. Residual Lead Remaining on Coupons After Sponge Cleaning Only Versus Surface Tension, by Substrate and Soil Types 7-15 ------- Table 7-10. Analysis of Covariance Results: Total Lead Accounted for in the Cleaning Process Dependent (response) variable Number of observations Root mean square error Mean response Factor Phosphate Substrate Soil bath Surface tension * phosphate Surface tension * substrate * soil type Log-transformed percentage of lead accounted for 127 (1 statistical outlier excluded) 0.1300 (corresponding to a coefficient of variation in the untransformed unit of 13.9 percent) 4.5738 (corresponding to a geometric mean in the untransformed unit of 96.9 percent) Degrees of freedom 3 1 1 3 3 Sum of squares 0.15 0.04 0.09 0.21 0.52 Mean square 0.05 0.04 0.09 0.07 0.17 F ratio 2.98 2.62 5.27 4.17 10.16 Prob>F 0.0344 0.1086 0.0235 0.0076 0.0001 Whole-model analysis of variance test Source Model Error Corrected total Degrees of freedom 12 114 126 Sum of squares 1.68 1.93 3.61 Mean square 0.14 0.02 F-ratio 8.29 Prob>F 0.0001 Overall, the geometric mean percentage lead accounted for was 96.9 percent with a confidence interval of 94.7 to 99.1 to percent. Thus, between 0.85 and 5.28 percent of the lead was unaccounted for. Based on the individual percentage of lead estimated in the analyses above, a similar mean total lead percentage was accounted for: • Sponge and wipe: 72.7 (sponge) + 1.47 (wipe) + 21.5 (coupon) = 95.6 percent • Sponge-cleaning only: 72.7 (sponge) + 24.2 (coupon) = 96.9 percent The slight differences among the three mass balance estimates resulted from the different factors and the different subsets of the data used in different analysis of covariance models. 7-16 ------- From this analysis, between 0.85 and 5.28 percent of the lead applied was unaccounted for. This small discrepancy could be due to several factors. One factor could be the estimation of the amount of lead applied. The estimation of the quantity of lead applied to the coupons was based on a small set of eight experiments (Section 6.2). As per recipe, the concentration of lead would be approximately 481 ug/mL in dry soil and 463 ug/mL of oily soil. The estimates from this study are 485.1 ug/mL (batch 1) and 491.7 ug/mL (batch 2) in dry soil; and 389.6 ug/mL (batch 1) and 475.2 fig/mL (batch 2) in oily soil. Three of these estimates are above recipe levels, while the fourth is well below recipe value. Thus, overestimating the amount applied could result in underestimating the percentage accounted for. Furthermore, as shown in Figures 5-1 and 5-2, lead recovery from coupons and sponges is in most cases well below 100 percent. Both coupons and sponges are two new and difficult matrices from which lead was extracted using Modified EPA Method 3050A. It is likely that the consistently low lead recovery from coupons and sponges also contributes to the deficit in mass balance. For completeness, mass balance results (on log-scale) were plotted versus surface tension, separately for the four combinations of substrate and soil types. These plots are shown in Figure 7-7. 7-17 ------- Enamel.Dry Enamel.Oily 5.2 3T s.o ? § 4.8 I4'6 J44 | 4.2 An i i i i i 0 0 o 0 °<> 0 ° - o o o 0 o o o ° °o 0 0 "" o — 1 - 1 1 . 1 1 20 30 40 50 60 70 80 Surface tension (dyne/cm) £ 1 I a $ to a a.i 5.0 4.8 4.6 4.4 4.2 An 0 0 - o - o o 00 0 -oo 0 ° 0 - o 1 1 1 1 1 20 30 40 50 60 70 80 Surface tension (dyne/cm) Latex.Dry Latex.Oily »M Mass balance (%) (lo Ik 4k. 4k 4k J 3 N> 4k b> C — r — i i i — r o o O rt O - °o ° °° o° - o 2*5.0 8 V 0» A A Mass balance (%) (lo Ik 4k 4k 4k J D K) 4k » i _ o o - ° 00 0°0 o 0 0 - o 0 ° - o O o o o o o ~ II ° L .1 20 30 40 50 60 70 80 Surface tension (dyne/cm) 20 30 40 50 60 70 80 Surface tension (dyne/cm) Figure 7-7. Total Percentage of Lead Accounted for Versus Surface Tension, by Substrate and Soil Types 7-18 ------- Section 8 References 1. Rogers, J., Hartley, W., and Cooper, G. Laboratory Study of Lead-Cleaning Efficacy. Report No. EPA 747-R-97-002. March 1997. 2. USEPA. July 12,1995. Quality Assurance Project Plan for Pb-Cleaning Efficacyfor Lead Abatement in Housing, Revision No. 4. Prepared under contract by Midwest Research Institute, Kansas City, MO. 3. Addition to QAPjP for Pb-Cleaning Efficacy for Lead Abatement in Housing, Revision No. 4, July 12,1995. Appendix B-l, Analytical Procedure Modified Method 3050A for Analysis of Lead (Pb) in Sponge Samples. 4. Addition to QAPjP for Pb-Cleaning Efficacy for Lead Abatement in Housing, Revision No. 4, July 12,1995. Appendix B-2, Analytical Procedure Modified Method 3050A for Analysis of Lead (Pb) in Core Samples. 8-1 ------- Appendix A Test Schedule ------- Table A-l (Continued) Soil batch 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 Measurement method Wipe Wipe Wipe Wipe Wipe No wipe No wipe No wipe No wipe Wipe Wipe Wipe Wipe No wipe No wipe No wipe No wipe Wipe Wipe Wipe Wipe No wipe No wipe No wipe No wipe No wipe No wipe No wipe No wipe Wipe Wipe Wipe Wipe No wipe No wipe No wipe No wipe Wipe Wipe Wipe Wipe Wipe Wipe Wipe Wine Cleaning solution 11 12 12 12 12 13 13 13 13 14 14 14 14 15 15 15 15 16 16 16 16 17 17 17 17 18 18 18 18 19 19 19 19 20 20 20 20 21 21 21 21 22 22 22 22 Surface Phosphate tension 30 40 40 40 40 70 70 70 70 60 60 60 60 60 60 60 60 30 30 30 30 70 70 70 70 40 40 40 40 40 40 40 40 70 70 70 70 40 40 40 40 Include 60 60 60 60 level 14 11 11 11 11 11 11 11 11 11 11 11 11 14 14 14 14 0 0 0 0 0 0 0 0 11 11 11 11 14 14 14 14 14 14 14 14 0 0 0 0 Soil type Oily Dry Oily Dry Oily Dry Dry Oily Oily Oily Oily Dry Dry Oily Oily Dry Dry Dry Oily Oily Dry Oily Dry Dry Oily Dry Oily Oily Dry Oily Oily Dry Dry Oily Dry Oily Dry Dry Dry Oily Oily precleaning test No. 5: 14 14 14 14 Dry Dry Oily Oitv Substrate Enamel Enamel Latex Latex Enamel Enamel Latex Latex Enamel Enamel Latex Latex Enamel Enamel Latex Latex Enamel Latex Latex Enamel Enamel Latex Enamel Latex Enamel Latex Enamel Latex Enamel Latex Enamel Latex Enamel Enamel Latex Latex Enamel Latex Enamel Enamel Latex dry soil batch Enamel Latex Enamel Latex Test sequence number 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 2 on latex 85 86 87 88 A-2 ------- Table A-l (Continued) Soil batch 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 Measurement method No wipe No wipe No wipe No wipe No wipe No wipe No wipe No wipe No wipe No wipe No wipe No wipe Wipe Wipe Wipe Wipe Wipe Wipe Wipe Wipe Wipe Wipe Wipe Wipe No wipe No wipe No wipe No wipe Cleaning solution 23 23 23 23 24 24 24 24 25 25 25 25 26 26 26 26 27 27 27 27 28 28 28 28 29 29 29 29 Surface tension Include 40 40 40 40 30 30 30 30 30 30 30 30 70 70 70 70 60 60 60 60 Include 30 30 30 30 60 60 60 60 Phosphate level Soil type precleaning test No. 6: 3 3 3 3 14 14 14 14 0 0 0 0 11 11 11 11 0 0 0 0 Dry Dry Oily Oily Dry Oily Dry Oily Oily Dry Dry Oily Oily Oily Dry Dry Oily Dry Dry Oily precleaning test No. 7: 3 3 3 3 3 3 3 3 Include precleaning Wipe Wipe Wipe Wipe No wipe No wipe No wipe No wipe Wipe Wipe Wipe Wine 30 30 30 30 31 31 31 31 32 32 32 32 70 70 70 70 60 60 60 60 30 30 30 30 3 3 3 3 11 11 11 11 11 11 11 11 Dry Oily Oily Dry Dry Oily Dry Oily test No. Oily Dry Oily Dry Dry Oily Oily Dry Oily Oily Dry Dry Substrate dry soil batch 2 Enamel Latex Latex Enamel Enamel Enamel Latex Latex Latex Latex Enamel Enamel Enamel Latex Enamel Latex Enamel Latex Enamel Latex Test sequence number on enamel 89 90 91 92 93 94 95 96 97 98 99 100 101 102 103 104 105 106 107 108 oily soil batch 2 on enamel Enamel Latex Enamel Latex Enamel Enamel Latex Latex 8: oily soil batch Enamel Enamel Latex Latex Latex Latex Enamel Enamel Enamel Latex Latex Enamel 109 110 111 112 113 114 115 116 2 on latex 117 118 119 120 121 122 123 124 125 126 127 128 A-3 ------- Appendix B Laboratory Data—Test and QC Samples ------- Laboratory data for 723 (test and laboratory QC) samples are presented in this appendix. Data for the 598 instrument QC samples are not shown here. The data are organized by analytical instrument file name (total of IS), and within each instrument file by analytical run number (i.e., analysis sequence). Page breaks occur after each instrumental file. The data tables were generated in SAS with the following headers: SAS variable name OBS MATRIX INSTRMNT PREFETCH RUN_NO QCJD LAB_ID SAMPLED) SUBSTRAT CLMDC SOILTYPE SO1LBTCH SMPLTYPE MIL C AMOUNT SRMREC Definition (unit} Running observation number (1 through 723) Matrix (wipe, sponge, core, liquid) Analytical instrument (ICP or GFAA) Analytical preparation batch number Analytical run number (starts over within each instrument file) QC ID code: Test, MB, MMB, LCS, or SRM Laboratory ID Sample ID; these relate to the coupons generated in the "test" (coupon preparation laboratory). The following 5 variables are subparts of mis variable. Substrate (enamel or latex) Cleaning solution number (01 through 32) Soil type (D=dry; L=oily) Soil batch number (1 or 2) Sample type (all Ws=wipe; CR=core; SP=sponge; RR=rod rinse) mL of soil applied to coupons (2 mL on enamel; 4 mL on latex) Comment indicating whether the amount of lead is below detection limit Total amount of lead per sample, in ug. Note that the amounts for core samples are not corrected for total soiled coupon surface. Percent recovery; applies to SRM and LCS only. B-l ------- FIELD AND QC LABORATORY DATA W to OBS 1 2 3 4 5 6 7 8 9 10 11 12 13 U 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 MATRIX WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE INSTRMNT ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP PREPBTCH 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-17 4816-17 4816-17 4816-17 4816-17 4816-17 4816-17 4816-17 4816-17 4816-17 4816-17 4816-17 4816-17 4816-17 4816-17 4816-17 4816-17 4816-17 4816-17 4816-17 4816-12 4816-12 4816-12 4816-12 4816-12 4816-12 4816-12 4816-12 4816-12 RUN_NO 23 24 25 26 27 28 29 30 31 32 38 39 40 41 42 43 44 45 46 47 53 54 55 56 57 58 59 60 61 62 70 71 72 73 74 75 76 77 78 79 85 86 87 88 89 90 91 92 93 94 102 103 104 QC_ID FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD LCS MMB SRM 2710 MB FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD SRM 2710 MMB MB LCS FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD LABJD 2280 2281 2282 2283 2284 2285 2286 2287 2288 2289 2290 2291 2292 2293 2294 2295 2296 2297 2326 2327 2386 2387 2401 DF5 2421 2330 2331 2335 2336 2340 2341 2345 2346 2350 2351 2355 2356 2360 2361 2365 2366 2437 DF5 2439 2440 2441 2298 2299 2300 2301 2302 2303 2304 2305 2306 •- lMLb=t SAMPLE ID PL12D1WW LF12D1WW PL12L1WW LF12L1WW PL14D1WW LF14D1WW PL14L1WW LF14L1WW PL16D1WW LF16D1WW PL16L1WW LF16L1WW PL16DOWW LF16DOWW PL19D2WW LF19D2WW PL19L2WW LF19L2WW PL32LOWW LF32LOWW LCS MMB SRM 2710 MB PCPLL1W1 PCPLL1W2 PCLFL1W1 PCLFL1W2 PCLFD1W1 PCLFD1W2 PCPLD1W1 PCPLD1W2 PCLFD2W1 PCLFD2W2 PCPLD2W1 PCPLD2W2 PCPLL2W1 PCPLL2W2 PCLFL2W1 PCLFL2W2 SRM 2710 MMB MB LCS PL21D2WW LF21D2WW PL21L2WW LF21L2WW PL22D2WW LF22D2WW PL22L2WW LF22L2WW PL2602WW .uouy/A - SUBSTRAT ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL ENAMEL LATEX LATEX LATEX LATEX ENAMEL ENAMEL LATEX LATEX ENAMEL ENAMEL ENAMEL ENAMEL LATEX LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL CLMIX 12 12 12 12 14 14 14 14 16 16 16 16 16 16 19 19 19 19 32 32 21 21 21 21 22 22 22 22 26 SOILTYPE D D L L D D L L D D I L D D D D I I L L L L L L D D D D D D D D L L L L D D L L D D L L D SOILBTCH 1 1 1 1 1 1 1 1 1 1 1 1 0 0 2 2 2 2 0 0 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 SMPLTYPE WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW W1 W2 W1 W2 W1 W2 W1 W2 W1 W2 W1 W2 W1 W2 W1 W2 WW WW WW WW WW WW WW WW WW MIL 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 2 4 4 4 4 2 2 4 4 2 2 2 2 4 4 2 4 2 4 2 4 2 4 2 C AMOUNT SRMREC 5.97 52.93 14.55 37.68 4.27 24.67 11.82 49.27 15.85 24.92 17.80 54.92 < 3.44 < 3.44 7.69 49.88 8.70 47.80 < 3.44 < 3.44 101.37 101 < 3.44 4394.75 78 < 3.44 641.24 16.51 1119.60 124.99 1399.90 63.50 759.86 21.04 1480.10 136.65 831.31 93.74 764.21 37.72 1549.10 126.30 5682.00 102 < 3.44 29.36 < 3.44 3 16.26 29.82 31.16 51.40 5.96 39.81 9.49 25.20 < 3.44 370 717 600 441 ------- CO u» FIELD AND QC LABORATORY DATA iriLe=tuouy'A (continued) DBS 54 55 56 57 58 59 60 61 62 MATRIX WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE INSTRNNT ICP ICP ICP ICP ICP ICP ICP ICP ICP PREPBTCH 4816-12 4816-12 4816-12 4816-12 4816-12 4816-12 4816-12 4816-12 4816-12 RUN_NO 105 106 107 108 109 115 116 117 118 QC_ID FIELD FIELD FIELD FIELD FIELD LCS SRH 2710 MMB MB LABJD 2307 2308 2309 2398 2399 2388 2430 DF5 2433 2434 SAMPLEID LF26D2WW PL26L2WW LF26L2WW LF12D1WW2 LF12L1WW2 LCS SRM 2710 MMB MB SUBSTRAT LATEX ENAMEL LATEX LATEX LATEX CLMIX 26 26 26 12 12 SOILTYPE D L L D L SOILBTCH 2 2 2 1 1 SMPLTYPE UW WW WW WW2 WW2 MIL 4 2 4 4 4 C AMOUNT 28.24 11.27 63.58 23.82 16.37 95.03 5925.50 < 3.44 < 3.44 SRMREC * • _ 95 i 026 106.881 . * ------- FIELD AND QC LABORATORY DATA W DBS 63 64 65 66 67 68 69 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 101 102 103 104 105 106 MATRIX WIPE WIPE WIPE WIPE UIPE WIPE UIPE WIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE UIPE INSTRHNT ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP PREPBTCH 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A RUNJK) 23 24 25 26 27 28 29 30 31 32 38 39 40 41 42 43 44 45 46 47 55 56 57 58 59 60 61 62 63 64 70 71 72 73 74 75 76 77 78 79 85 86 87 88 QCJD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD MHB SRN 2710 LCS MB FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD LCS MMB SRH 2710 MB LABJD 2310 2311 2312 2313 2314 2315 2316 2317 2318 2319 2320 2321 2322 2323 2324 2325 2389 2431 DF5 2435 2436 2260 2261 2262 2263 2264 2265 2266 2267 2268 2269 2270 2271 2272 2273 2274 2275 2276 2277 2278 2279 2384 2385 2402 DF5 2420 •- IFILE-I SAMPLEID PL27D2UU LF27D2UU PL27L2UU LF27L2UU PL28D2UU LF28D2UU PL28L2UU LF28L2UU PL30D2UU LF30D2UU PL30L2UU LF30L2UU PL32D2UU LF32D2UU PL32L2UU LF32L2UU HUB SRH 2710 LCS MB PL01D1UU LF01D1WW PL01L1UU LF01L1UU PL03D1WU LF03D1UU PL03L1UU LF03L1UU PL05D1UU LF05D1UU PL05L1UU LF05L1UU PL06D1UU LF06D1UU PL06L1UU LF06L1UU PL11D1UU LF11D1UU PL11L1UU LF11L1UU LCS MMB SRM 2710 MB :DBWA -• SUBSTRAT ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX CLMIX 27 27 27 27 28 28 28 28 30 30 30 30 32 32 32 32 01 01 01 01 03 03 03 03 05 05 05 05 06 06 06 06 11 11 11 11 SOILTYPE D D L L D D L L D D I L D D L L D D L L D D L L D D L L D D L L D D L L SOILBTCH 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 1 1 1 1 1 1 1 1 1 SMPLTYPE WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW MIL 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 C AMOUNT SRMREC 15.38 46.10 27.89 67.70 3.13 18.89 13.49 35.41 6.07 24.73 12.64 24.85 4.33 18.80 4.60 19.64 2.46 5222.50 94 93.11 93 < 2.24 12.57 32.08 27.85 61.67 12.80 55.55 33.57 47.47 10.01 59.73 19.15 46.20 6.29 49.21 13.77 66.45 4.88 37.57 8.86 21.41 98.68 98 < 2.24 5303.00 95 < 2.24 2009 1130 6790 4807 ------- FIELD AND QC LABORATORY DATA Cd DBS NATRIX 107 SPONGE 108 SPONGE 109 SPONGE 110 SPONGE 111 SPONGE 112 SPONGE 113 SPONGE 114 SPONGE 115 SPONGE 116 SPONGE 117 SPONGE 118 SPONGE 119 SPONGE 120 SPONGE 121 SPONGE 122 SPONGE 123 SPONGE 124 SPONGE 125 SPONGE 126 SPONGE 127 SPONGE 128 SPONGE 129 SPONGE 130 SPONGE 131 SPONGE 132 SPONGE 133 SPONGE 134 SPONGE 135 SPONGE 136 SPONGE 137 SPONGE 138 SPONGE 139 SPONGE 140 SPONGE 141 SPONGE 142 SPONGE 143 SPONGE 144 SPONGE 145 SPONGE 146 SPONGE 147 SPONGE 148 SPONGE 149 SPONGE 150 SPONGE 151 SPONGE 152 SPONGE 153 SPONGE 154 SPONGE 155 SPONGE 156 SPONGE 157 SPONGE 158 SPONGE 159 SPONGE INSTRMNT ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP PREPBTCH 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-16 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-11 4816-5 4816-5 4816-5 4816-5 4816-5 RUN_NO QCJD 23 FIELD 24 FIELD 25 FIELD 26 FIELD 27 FIELD 28 FIELD 29 FIELD 30 FIELD 31 FIELD 32 FIELD 38 FIELD 39 FIELD 40 FIELD 41 FIELD 42 FIELD 43 FIELD 44 FIELD 45 FIELD 46 FIELD 47 FIELD 55 HUB 56 LCS 57 SRH 2710 58 MB 59 FIELD 60 FIELD 61 FIELD 62 FIELD 63 FIELD 64 FIELD 70 FIELD 71 FIELD 72 FIELD 73 FIELD 74 FIELD 75 FIELD 76 FIELD 77 FIELD 78 FIELD 79 FIELD 87 FIELD 88 FIELD 89 FIELD 90 FIELD 91 LCS 92 HUB 93 SRN 2710 94 MB 95 FIELD 96 FIELD 102 FIELD 103 FIELD 104 FIELD LAB_ID 2028 2029 2030 2031 2032 2033 2034 2035 2036 2037 2038 2039 2040 2041 2042 2043 2044 2045 2046 2047 2405 2406 2407 DF5 2438 2008 2009 2010 2011 2012 2013 2014 2015 2016 2017 2018 2019 2020 2021 2022 2023 2024 2025 2026 2027 2371 2403 2404 DF5 2432 1988 1989 1990 1991 1992 iriLC^cuoiorn RUN SAMPLE ID SUBSTRAT PL11D1SP ENAMEL LF11D1SP LATEX PL11L1SP ENAMEL LF11L1SP LATEX PL12D1SP ENAMEL LF12D1SP LATEX PL12L1SP ENAMEL LF12L1SP LATEX PL13D1SP ENAMEL LF13D1SP LATEX PL13L1SP ENAMEL LF13L1SP LATEX PL14D1SP ENAMEL LF14D1SP LATEX PL14L1SP ENAMEL LF14L1SP LATEX PL15D1SP ENAMEL LF15D1SP LATEX PL15L1SP ENAMEL LF15L1SP LATEX MMB LCS SRM 2710 MB PL06D1SP ENAMEL LF06D1SP LATEX PL06L1SP ENAMEL LF06L1SP LATEX PL07D1SP ENAMEL LF07D1SP LATEX PL07L1SP ENAMEL LF07L1SP LATEX PL08D1SP ENAMEL LF08D1SP LATEX PL08L1SP ENAMEL LF08L1SP LATEX PL09D1SP ENAMEL LF09D1SP LATEX PL09L1SP ENAMEL LF09L1SP LATEX PL10D1SP ENAMEL LF10D1SP LATEX PL10L1SP ENAMEL LF10L1SP LATEX LCS MMB SRM 2710 MB PL01D1SP ENAMEL LF01D1SP LATEX PL01L1SP ENAMEL LF01L1SP LATEX PL02D1SP ENAMEL CLMIX 11 11 11 11 12 12 12 12 13 13 13 13 14 14 14 14 15 15 15 15 06 06 06 06 07 07 07 07 08 08 08 08 09 09 09 09 10 10 10 10 01 01 01 01 02 SOILTYPE SOILBTCH SMPLTYPE D D L L D D L L D D L L D D L L D D L I D D | L o o • L D D L L D D L L D D L I 1 D 1 D 1 L 1 L 1 D 1 1 SP 1 SP 1 SP 1 SP 1 SP SP SP SP SP SP SP SP SP 1 SP 1 SP 1 SP 1 SP 1 SP 1 SP 1 SP 1 SP 1 SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP MIL 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 C AMOUNT SRMREC 572.61 1135.80 549.20 872.28 696.63 1281.40 596.00 904.09 651.28 1177.80 507.92 668.93 514.53 1492.10 676.96 1063.70 665.18 1297.40 653.78 1076.20 2.98 94.06 94 5248.00 94 < 2.65 611.45 1193.40 514.62 925.00 753.07 1286.60 604.65 1130.10 688.82 1260.40 583.39 687.69 726.32 1247.90 751.93 1180.00 773.54 1605.70 674.43 1068.30 100.12 100 3.37 5285.00 94 < 2.65 663.43 1397.90 587.65 1013.00 713.29 062 473 120 798 ------- FIELD AND QC LABORATORY DATA CO O\ 1(.j Lt=tUO lOfft KUN 1 -- (continued) DBS MATRIX INSTRMNT PREPBTCH 160 SPONGE 161 SPONGE 162 SPONGE 163 SPONGE 164 SPONGE 165 SPONGE 166 SPONGE 167 SPONGE 168 SPONGE 169 SPONGE 170 SPONGE 171 SPONGE 172 SPONGE 173 SPONGE 174 SPONGE 175 SPONGE 176 SPONGE 177 SPONGE 178 SPONGE ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP 4816-5 4816-5 4816-5 4816-5 4816-5 4816-5 4816-5 4816-5 4816-5 4816-5 4816-5 4816-5 4816-5 4816-5 4816-5 4816-5 4816-5 4816-5 4816-5 RUN_NO 105 106 107 108 109 110 111 119 120 121 122 123 124 125 126 132 133 134 135 QC_ID FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD SRM 2710 HUB LCS MB LABJD 1993 1994 1995 1996 1997 1998 1999 2000 2001 2002 2003 2004 2005 2006 2007 2368 DF5 2369 2370 2400 SAMPLE ID LF02D1SP PL02L1SP LF02L1SP PL03D1SP LF03D1SP PL03L1SP LF03L1SP PL04D1SP LF04D1SP PL04L1SP LF04L1SP PL05D1SP LF05D1SP PL05L1SP LF05L1SP SRM 2710 MMB LCS MB SUBSTRAT LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX CLMIX 02 02 02 03 03 03 03 04 04 04 04 05 05 05 05 SOILTYPE D L L D D L L D D L L D D L L SOILBTCH SMPLTYPE MIL 1 SP 1 SP 1 SP 1 SP 1 SP 1 SP 1 SP 1 SP 1 SP 1 SP 1 SP 1 SP 1 SP 1 SP 1 SP 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 C AMOUNT SRMREC 1402.00 566.32 1107.70 669.41 1062.50 610.01 1186.90 931.32 1342.10 646.82 1151.50 868.78 1549.80 633.83 1230.30 5138.50 92 2.96 99.60 99 3.28 5522 5990 ------- FIELD AND QC LABORATORY DATA C0 OBS MATRIX 179 SPONGE 180 SPONGE 181 SPONGE 182 SPONGE 183 SPONGE 184 SPONGE 185 SPONGE 186 SPONGE 187 SPONGE 188 SPONGE 189 SPONGE 190 SPONGE 191 SPONGE 192 SPONGE 193 SPONGE 194 SPONGE 195 SPONGE 196 SPONGE 197 SPONGE 198 SPONGE 199 SPONGE 200 SPONGE 201 SPONGE 202 SPONGE 203 SPONGE 204 SPONGE 205 SPONGE 206 SPONGE 207 SPONGE 208 SPONGE 209 SPONGE 210 SPONGE 211 SPONGE 212 SPONGE 213 SPONGE 214 SPONGE 215 SPONGE 216 SPONGE 217 SPONGE 218 SPONGE 219 SPONGE 220 SPONGE 221 SPONGE 222 SPONGE 223 SPONGE 224 SPONGE 225 SPONGE 226 SPONGE INSTRMNT ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP PREPBTCH 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 4816-24 RUN_NO 24 25 26 27 28 29 30 31 32 33 39 40 41 42 43 44 45 46 47 48 54 55 56 57 58 59 60 61 62 63 71 72 73 74 75 76 77 78 79 80 86 87 88 89 90 91 92 93 QCJD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD MHB LCS SRM 2710 MB FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD LCS SRM 2710 MMB MB LAB_ID 2048 2049 2050 2051 2052 2053 2054 2055 2056 2057 2058 2059 2060 2061 2062 2063 2064 2065 2066 2067 2408 2416 2418 DF5 2445 2068 2069 2070 2071 2072 2073 2074 2075 2076 2077 2078 2079 2080 2081 2082 2083 2084 2085 2086 2087 2413 2415 DF5 2417 2446 1 1- 1 Lt=tUB SAMPLEID PL16D1SP LF16D1SP PL16L1SP LF16L1SP PL16DOSP LF16DOSP PL16LOSP LF16LOSP PL17D2SP LF17D2SP PL17L2SP LF17L2SP PL18D2SP LF18D2SP PL18L2SP LF18L2SP PL19D2SP LF19D2SP PL19L2SP LF19L2SP MMB LCS SRM 2710 MB PL20D2SP LF20D2SP PL20L2SP LF20L2SP PL21D2SP LF21D2SP PL21L2SP LF21L2SP PL22D2SP LF22D2SP PL22L2SP LF22L2SP PL23D2SP LF23D2SP PL23L2SP LF23L2SP PL24D2SP LF24D2SP PL24L2SP LF24L2SP LCS SRM 2710 MMB MB IOfA KUN < SUBSTRAT ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX £ CLMIX 16 16 16 16 16 16 16 16 17 17 17 17 18 18 18 18 19 19 19 19 20 20 20 20 21 21 21 21 22 22 22 22 23 23 23 23 24 24 24 24 SOILTYPE D D L L D D I L D D L L D D L L D D L L D D L L D D L L D D L L D D L L D D L L SOILBTCH 1 1 1 1 0 0 0 0 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 SMPLTYPE SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP MIL 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 C AMOUNT SRMREC 742.34 1364.80 605.81 1131.30 128.68 < 7.39 < 7.39 11.73 725.49 1335.10 775.09 1145.40 756.66 1346.40 751.23 1316.90 761.99 1420.30 811.38 1415.10 20.99 91.26 91 5369.50 96 < 7.39 699.03 1316.80 668.26 1137.60 755.74 1341.30 732.92 1146.90 589.31 1381.80 783.91 1162.70 705.38 1399.10 723.76 1280.70 666.97 1373.90 740.42 1181.60 88.41 88 5455.50 98 < 7.39 < 7.39 2590 5043 4090 4925 ------- FIELD AND QC LABORATORY DATA CO 00 DBS MATRIX 227 SPONGE 228 SPONGE 229 SPONGE 230 SPONGE 231 SPONGE 232 SPONGE 233 SPONGE 234 SPONGE 235 SPONGE 236 SPONGE 237 SPONGE 238 SPONGE 239 SPONGE 240 SPONGE 241 SPONGE 242 SPONGE 243 SPONGE 244 SPONGE 245 SPONGE 246 SPONGE 247 SPONGE 248 SPONGE 249 SPONGE 250 SPONGE 251 SPONGE 252 SPONGE 253 SPONGE 254 SPONGE 255 SPONGE 256 SPONGE 257 SPONGE 258 SPONGE 259 SPONGE 260 SPONGE 261 SPONGE 262 SPONGE 263 SPONGE 264 SPONGE 265 SPONGE 266 SPONGE 267 SPONGE 268 SPONGE 269 SPONGE 270 SPONGE INSTRNNT ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP PREPBTCH 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-29 4816-34 4816-34 4816-34 4816-34 4816-34 4816-34 4816-34 4816-34 4816-34 4816-34 4816-34 4816-34 4816-34 4816-34 4816-34 4816-34 4816-34 4816-34 4816-34 4816-34 RUN_NO 55 56 57 58 59 60 61 62 70 71 72 73 74 75 76 77 78 79 85 86 87 88 89 90 91 92 93 94 100 101 102 103 104 105 106 107 108 114 115 116 117 118 119 120 QC_ID LABJD FIELD 2088 FIELD 2089 FIELD 2090 FIELD 2091 FIELD 2092 FIELD 2093 FIELD 2094 FIELD 2095 FIELD 2096 FIELD 2097 FIELD 2098 FIELD 2099 FIELD 2100 FIELD 2101 FIELD 2102 FIELD 2103 FIELD 2104 FIELD 2105 FIELD 2106 FIELD 2107 HMB 2409 LCS 2412 SRM 2710 2419 DF5 MB 2449 FIELD 2108 FIELD 2109 FIELD 2110 FIELD 2111 FIELD 2112 FIELD 2113 FIELD 2114 FIELD 2115 FIELD 2116 FIELD 2117 FIELD 2118 FIELD 2119 FIELD 2120 FIELD 2121 FIELD 2122 FIELD 2123 MMB 2410 SRM 2710 2411 DF5 SRM 2710 2414 DF5 MB 2453 -- IFILE=I SAMPLEID PL25D2SP LF25D2SP PL25L2SP LF25L2SP PL26D2SP LF26D2SP PL26L2SP LF26L2SP PL27D2SP LF27D2SP PL27L2SP LF27L2SP PL28D2SP LF28D2SP PL28L2SP LF28L2SP PL29D2SP LF29D2SP PL29L2SP LF29L2SP MMB LCS SRM 2710 MB PL30D2SP LF30D2SP PL30L2SP LF30L2SP PL31D2SP LF31D2SP PL31L2SP LF31L2SP PL32D2SP LF32D2SP PL32L2SP LF32L2SP PL32DOSP LF32DOSP PL32LOSP LF32LOSP MHB SRM 2710 SRM 2710 MB :UBlB/« - SUBSTRAT ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX CLMIX 25 25 25 25 26 26 26 26 27 27 27 27 28 28 28 28 29 29 29 29 30 30 30 30 31 31 31 31 32 32 32 32 32 32 32 32 SOILTYPE D D L L D D L L D D L L D D L L D D L L D D L L D D I L D D L L D D L L SOILBTCH 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 0 0 0 0 SMPLTYPE SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP . SP SP SP SP SP SP SP SP SP SP SP SP SP SP SP MIL 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 C AMOUNT SRMREC 411.19 1178.00 473.50 1135.90 717.80 1335.20 643.87 742.64 639.91 1342.60 673.94 589.83 670.01 1482.60 736.71 1406.50 724.01 1469.60 688.27 1315.80 130.13 82.81 82 5763.50 103 < 3.40 637.36 1590.80 744.25 1340.10 645.62 1322.50 680.40 1363.40 728.28 1406.00 769.57 1239.30 < 3.40 < 3.40 11.02 70.63 < 3.40 5541.50 99 5211.50 93 < 3.40 809 884 363 715 ------- FIELD AND QC LABORATORY DATA W DBS 271 272 273 274 275 276 277 278 279 280 281 282 283 284 285 286 287 288 289 290 291 292 293 294 295 296 297 298 299 300 301 302 303 304 305 306 307 308 309 310 311 312 313 314 315 316 317 318 319 320 321 322 323 MATRIX CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE INSTRMNT ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP PREPBTCH 4816-18 4816-18 4816-18 4816-18 4816-18 •4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-21 4816-21 4816-21 4816-21 4816-21 RUN_NO 23 24 25 26 27 28 29 30 31 32 38 39 40 41 42 43 44 45 46 47 53 54 55 56 57 58 59 60 61 62 70 71 72 73 74 75 76 77 78 79 85 86 87 88 89 90 91 92 93 94 102 103 104 QC_ID FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD LCS SRM 2710 HUB MB FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD SRM 2710 HUB LCS MB FIELD FIELD FIELD FIELD FIELD LABJD 2124 2125 2126 2127 2128 2129 2130 2131 2132 2133 2134 2135 2136 2137 2138 2139 2140 2141 2142 2143 2379 2394 DF5 2424 2442 2144 2145 2146 2147 2148 2149 2150 2151 2152 2153 2154 2155 2156 2157 2158 2159 2160 2161 2162 2163 2376 DF5 2393 2428 2443 2164 2165 2166 2167 2168 SAMPLEID PL01D1CR LF01D1CR PL01L1CR LF01L1CR PL02D1CR LF02D1CR PL02L1CR LF02L1CR PL03D1CR LF03D1CR PL03L1CR LF03L1CR PL04D1CR LF04D1CR PL04L1CR LF04L1CR PL05D1CR LF05D1CR PL05L1CR LF05L1CR LCS SRN 2710 MMB MB PL06D1CR LF0601CR PL06L1CR LF06L1CR PL07D1CR LF07D1CR PL07L1CR LF07L1CR PL0801CR LF0801CR PL08L1CR LF08L1CR PL09D1CR LF09D1CR PL09L1CR LF09L1CR PL10D1CR LF1001CR PL10L1CR LF10L1CR SRM 2710 MMB LCS MB PL11D1CR LF11D1CR PL11L1CR LF11L1CR PL12D1CR SUBSTRAT ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL CLMIX 01 01 01 01 02 02 02 02 03 03 03 03 04 04 04 04 05 05 05 05 06 06 06 06 07 07 07 07 08 08 08 08 09 09 09 09 10 10 10 10 11 11 11 11 12 SOILTYPE D D L L D D L L D D L L D D L L D D L I D D L L D D L L D D L L D D L L D D L I D D I L D SOILBTCH 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 SMPLTYPE CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR MIL 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 C AMOUNT SRMREC 6.93 7.08 8.48 8.07 4.59 7.13 6.18 6.58 5.53 9.44 6.32 7.15 6.89 7.56 4.88 5.08 4.16 11.13 6.23 6.72 85.98 86 5240.50 94 7.14 < 3.73 4.37 10.12 13.20 7.32 6.55 8.28 5.17 8.15 8.02 11.49 6.82 9.78 5.09 15.28 6.41 9.96 6.79 7.55 11.63 13.78 4578.35 82 5.55 85.63 85 4.15 6.09 7.59 6.61 5.48 7.43 0 6 4 6 ------- FIELD AND QC LABORATORY DATA CO i—i O IFILE=E08227A (continued) DBS MATRIX INSTRMMT PREPBTCH RUM_NO QC_ID LAB_ID SAHPLEID SUBSTRAT CLMIX SOILTYPE SOILBTCH SHPLTYPE MIL C AMOUNT SRMREC 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 0 0 0 0 2 2 2 2 2 2 2 2 2 2 2 2 324 325 326 327 328 329 330 331 332 333 334 335 336 337 338 339 340 341 342 343 344 345 346 347 348 349 350 351 352 353 354 355 356 357 358 359 360 361 362 363 364 365 366 CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 105 106 107 108 109 110 111 117 118 119 120 121 122 123 124 125 126 132 133 134 135 136 137 138 139 140 141 148 149 150 151 152 153 154 155 156 157 162 163 164 165 166 167 FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD LCS MMB SRM 2710 MB FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD MMB SRM 2710 LCS MB 2169 2170 2171 2172 2173 2174 2175 2176 2177 2178 2179 2180 2181 2182 2183 2396 2426 2429 DF5 2444 2184 2185 2186 2187 2188 2189 2190 2191 2192 2193 2194 2195 2196 2197 2198 2199 2200 2201 2202 2203 2381 2382 DF5 2383 2447 LF12D1CR PL12L1CR LF12L1CR PL13D1CR LF13D1CR PL13L1CR LF13L1CR PL14D1CR LF14D1CR PL14L1CR LF14L1CR PL15D1CR LF15D1CR PL15L1CR LF15L1CR LCS MMB SRM 2710 MB PL16D1CR LF16D1CR PL16L1CR LF16L1CR PL16DOCR LF16DOCR PL16LOCR LF16LOCR PL17D2CR LF17D2CR PL17L2CR LF17L2CR PL18D2CR LF18D2CR PL18L2CR LF18L2CR PL19D2CR LF19D2CR PL19L2CR LF19L2CR MMB SRM 2710 LCS MB LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX 12 12 12 13 13 13 13 14 14 14 14 15 15 15 15 16 16 16 16 16 16 16 16 17 17 17 17 18 18 18 18 19 19 19 19 D L L D D L L D D L L D D L L D D L L D D I L D D L L D D L L D D L L CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 7.49 7.81 6.24 6.04 8.99 5.46 11.76 8.71 8.34 6.23 9.53 5.80 9.39 5.08 12.03 91.61 91 7.34 4855.45 87 5.24 5.89 6.40 4.36 6.89 4.17 6.79 < 3.73 4.91 4.85 8.38 5.61 10.32 4.84 9.11 6.28 8.37 9.30 6.78 7.05 8.07 5.19 5271.00 95 89.33 89 < 3.73 ------- FIELD AND QC LABORATORY DATA 10 ttJ DBS MATRIX 367 LIQUID 368 LIQUID 369 LIQUID 370 LIQUID 371 LIQUID 372 LIQUID 373 LIQUID 374 LIQUID 375 LIQUID 376 LIQUID 377 LIQUID 378 LIQUID 379 LIQUID 380 LIQUID 381 LIQUID 382 LIQUID 383 LIQUID 384 LIQUID 385 LIQUID 386 LIQUID 387 CORE 388 CORE 389 CORE 390 CORE 391 CORE 392 CORE 393 CORE 394 CORE 395 CORE 396 CORE 397 CORE 398 CORE 399 CORE 400 CORE 401 CORE 402 CORE 403 CORE 404 CORE 405 CORE 406 CORE 407 CORE 408 CORE 409 CORE 410 CORE 411 CORE 412 CORE 413 CORE 414 CORE 415 CORE 416 CORE 417 CORE 418 CORE 419 CORE INSTRMNT ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP PREPBTCH 4816-37 4816-37 4816-37 4816-37 4816-37 4816-37 4816-37 4816-37 4816-37 4816-37 4816-37 4816-37 4816-37 4816-37 4816-37 4816-37 4816-37 4816-37 4816-37 4816-37 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 RUN.NO 23 24 25 26 27 28 29 30 31 32 38 39 40 41 42 43 44 45 46 47 55 56 57 58 59 60 61 62 63 64 70 71 72 73 74 75 76 77 78 79 85 86 87 88 89 90 91 92 93 94 102 103 104 QC_ID FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD SRN 2710 LCS MMB MB FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD LCS SRM 2710 MMB MB FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD LABJD 2328 2329 2333 2334 2338 2339 2343 2344 2348 DF2 2349 2353 2354 2358 2359 2363 2364 2454 DF5 2455 2456 2457 2204 2205 2206 2207 2208 2209 2210 2211 2212 2213 2214 2215 2216 2217 2218 2219 2220 2221 2222 2223 2391 2392 DF5 2395 2448 2224 2225 2226 2227 2228 2229 2230 2231 2232 SAMPLEID 2PCPLL1 PCPLL1RR 4PCLFL1 PCLFL1RR 4PCLFD1 PCLFD1RR 2PCPLD1 PCPLD1RR 4PCLFD2 PCLFD2RR 2PCPLD2 PCPLD2RR 2PCPLL2 PCPLL2RR 4PCLFL2 PCLFL2RR SRM 2710 LCS MMB MB PL20D2CR LF20D2CR PL20L2CR LF20L2CR PL21D2CR LF21D2CR PL21L2CR LF21L2CR PL22D2CR LF22D2CR PL22L2CR LF22L2CR PL23D2CR LF23D2CR PL23L2CR LF23L2CR PL24D2CR LF24D2CR PL24L2CR LF24L2CR LCS SRM 2710 MMB MB PL25D2CR LF25D2CR PL25L2CR LF25L2CR PL26D2CR LF26D2CR PL26L2CR LF26L2CR PL27D2CR SUBSTRAT ENAMEL ENAMEL LATEX LATEX LATEX LATEX ENAMEL ENAMEL LATEX LATEX ENAMEL ENAMEL ENAMEL ENAMEL LATEX LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL CLMIX 20 20 20 20 21 21 21 21 22 22 22 22 23 23 23 23 24 24 24 24 25 25 25 25 26 26 26 26 27 SOILTYPE L L L L D D D D D D D D L L L L D D L L D D L L D D L L D D L L D D L L D D L L D D L L D SOILBTCH 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 SMPLTYPE RR RR RR RR RR RR RR RR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR MIL 2 2 4 4 4 4 2 2 4 4 2 2 2 2 4 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 C AMOUNT SRMREC 783.50 20.09 1550.10 52.83 1931 .40 61.33 974.70 33.68 2004.60 42.34 964.72 26.26 909.29 20.03 1987.00 70.21 5055.50 90 86.62 86 < 2.38 < 2.38 < 2.38 4.46 < 2.38 7.45 18.26 2.80 2.75 4.68 < 2.38 3.89 < 2.38 3.41 2.78 5.72 6.83 5.60 < 2.38 3.29 4.48 3.68 89.34 89 4972.60 89 < 2.38 2.58 < 2.38 5.15 2.88 5.51 2.59 7.21 3.15 4.69 < 2.38 7304 6190 3400 8068 ------- FIELD AND QC LABORATORY DATA 11 Cd »«-i to IFILE=E09087A (continued) OBS MATRIX INSTRMNT PREPBTCH RUN NO QC ID LAB ID SAMPLEID SUBSTRAT CLHIX SOILTYPE SOILBTCH SMPLTYPE MIL C AMOUNT SRMREC 2 2 2 2 2 2 2 2 2 2 2 420 421 422 423 424 425 426 427 428 429 430 431 432 433 434 435 436 437 438 439 440 441 442 443 444 445 446 447 448 449 450 451 452 453 454 455 456 457 458 459 460 461 462 463 464 465 466 CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-31 4816-32 4816-32 4816-32 4816-32 4816-32 4816-32 4816-32 4816-32 105 106 107 108 109 110 111 117 118 119 120 121 122 123 124 125 126 134 135 136 137 138 139 140 141 142 143 148 149 150 151 1^2 153 154 155 15(S 157 162 163 164 165 166 167 168 169 170 171 FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD SRM 2710 LCS MMB MB FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD SRH 2710 LCS MMB MB FIELD FIELD FIELD FIELD LCS MMB SRM 2710 MB 2233 2234 2235 2236 2237 2238 2239 2240 2241 2242 2243 2380 DF5 2397 2425 2450 2244 2245 2246 2247 2248 2249 2250 2251 2252 2253 2254 2255 2256 2257 2258 2259 2332 2337 2342 2347 2378 DF5 2390 2423 2451 2352 2357 2362 2367 2377 2422 2427 DF5 2452 LF27D2CR PL27L2CR LF27L2CR PL28D2CR LF28D2CR PL28L2CR LF28L2CR PL29D2CR LF29D2CR PL29L2CR LF29L2CR SRM 2710 LCS MMB MB PL30D2CR LF30D2CR PL30L2CR LF30L2CR PL31D2CR LF31D2CR PL31L2CR LF31L2CR PL32D2CR LF32D2CR PL32L2CR LF32L2CR PL32DOCR LF32DOCR PL32LOCR LF32LOCR PCPLL1CR PCLFL1CR PCLFD1CR PCPLD1CR SRM 2710 LCS MMB MB PCLFD2CR PCPLD2CR PCPLL2CR PCLFL2CR LCS MMB SRM 2710 MB LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX LATEX ENAMEL LATEX ENAMEL ENAMEL LATEX 27 27 27 28 28 28 28 29 29 29 29 30 30 30 30 31 31 31 31 32 32 32 32 32 32 32 32 D L L D D L L D D L L D D L L D D L L D D L L D D L L L L D D D D L L CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 4 2 4 2 2 4 3.23 4.34 5.83 5.63 3.88 3.83 5.27 2.84 8.11 5.49 6.39 5247.50 94 74.30 74 9.21 < 2.38 3.09 5.39 3.62 4.36 2.47 6.77 3.19 7.62 3.14 5.00 4.79 3.84 4.70 3.36 2.97 3.17 4.30 4.69 7.21 8.70 5170.50 92 76.39 76 9.67 3.71 5.29 4.50 5.43 4.18 81.27 81 6.40 5113.50 92 < 2.38 3795 3010 6115 3900 2720 4015 ------- FIELD AND QC LABORATORY DATA 12 td DBS 467 468 469 470 471 472 473 474 475 476 477 478 479 480 481 482 483 484 485 486 487 488 489 490 MATRIX CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE INSTRMNT PREPBTCH GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-21 4816-25 RUN_NO QCJD 12 13 14 15 16 17 19 22 23 24 25 26 28 29 30 31 34 35 37 38 39 40 41 42 FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD LCS MMB MB FIELD iriLC= LABJD SAMPLEID 2164 2165 2166 2167 2168 2169 2170 2171 2172 2173 2174 2175 2176 2177 2178 2179 2180 2181 2182 2183 2396 2426 2444 2184 PL11D1CR LF11D1CR PL11L1CR LF11L1CR PL12D1CR LF12D1CR PL12L1CR LF12L1CR PL13D1CR LF13D1CR PL13L1CR LF13L1CR PL14D1CR LF14D1CR PL14L1CR LF14L1CR PL15D1CR LF15D1CR PL15L1CR LF15L1CR LCS MMB MB PL16D1CR vuyuorn. SUBSTRAT ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL ri CLMIX 11 11 11 11 12 12 12 12 13 13 13 13 14 14 14 14 15 15 15 15 16 SOILTYPE SOILBTCH SMPLTYPE MIL C AMOUNT SRMREC D D L L D D L L D D L L D D L L D D . L L D 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 4 2 2.90 4.65 3.02 3.07 3.90 3.26 2.89 4.91 2.32 4.79 2.40 6.15 3.33 3.79 3.08 5.08 1.88 4.94 1.92 5.61 80.50 80 2.38 : 0.06 1.16 5 ------- FIELD AND QC LABORATORY DATA 13 I £ DBS 491 492 493 494 495 496 497 498 499 500 501 502 503 504 505 506 507 508 509 510 511 512 513 514 515 516 517 518 519 520 521 522 523 524 525 526 527 528 529 530 531 532 533 534 535 536 MATRIX CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE INSTRMN1 GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA PREPBTCH 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-18 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 4816-20 RUN_NC 12 13 14 15 16 17 19 20 23 24 25 26 28 29 30 31 32 35 37 38 39 40 41 42 44 47 48 49 50 51 53 54 55 56 59 60 64 65 66 67 68 69 70 71 72 75 1 QC_ID FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD LCS MMB MB FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD MMB LCS MB LABJD 2124 2125 2126 2127 2128 2129 2130 2131 2132 2133 2134 2135 2136 2137 2138 2139 2140 2141 2142 2143 2379 2424 2442 2144 2145 2146 2147 2148 2149 2150 2151 2152 2153 2154 2155 2156 2157 2158 2159 2160 2161 2162 2163 2393 2428 2443 SAMPLEID PL01D1CR LF01D1CR PL01L1CR LF01L1CR PL02D1CR LF02D1CR PL02L1CR LF02L1CR PL03D1CR LF03D1CR PL03L1CR LF03L1CR PL04D1CR LF04D1CR PL04L1CR LF04L1CR PL05D1CR LF05D1CR PL05L1CR LF05L1CR LCS MMB MB PL06D1CR LF06D1CR PL06L1CR LF06L1CR PL07D1CR LF07D1CR PL07L1CR LF07L1CR PL08D1CR LF08D1CR PL08L1CR LF08L1CR PL09D1CR LF09D1CR PL09L1CR LF09L1CR PL10D1CR LF10D1CR PL10L1CR LF10L1CR MMB LCS MB vuyutsrA.i SUBSTRAT ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX •i CLMIX 01 01 01 01 02 02 02 02 03 03 03 03 04 04 04 04 05 05 05 05 06 06 06 06 07 07 07 07 08 08 08 08 09 09 09 09 10 10 10 10 S01LTYPE SOILBTCH D D L L D D L L 1 D 1 D 1 L 1 L 1 D 1 D 1 L 1 L 1 D 1 D 1 L 1 L 1 D 1 D 1 L 1 L 1 D 1 D 1 L 1 L 1 D 1 D 1 L 1 L 1 D 1 D 1 L 1 L 1 D 1 D 1 L 1 L 1 SMPLTYP CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR E MIL 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 : AMOUNT SRMREC 2.66 4.41 4.60 5.45 2.39 3.05 3.19 3.44 2.83 5.18 2.89 3.86 2.74 4.18 3.65 2.37 1.70 4.91 3.11 3.11 96.00 96 2.37 0.34 1.67 7.64 7.54 3.53 5.17 4.35 2.82 3.15 3.83 6.40 3.02 6.01 2.76 12.07 3.33 6.15 3.46 5.02 7.44 7.56 2.76 86.00 86 0.89 ------- FIELD AND QC LABORATORY DATA 1* W OBS 537 538 539 540 541 542 543 544 545 546 547 548 549 550 551 552 553 554 555 556 557 558 MATRIX CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE INSTRHNT PREPBTCH GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 4816-25 RUNJIO QC_ID 12 13 14 16 17 18 20 23 24 26 27 28 30 31 34 36 37 38 40 41 42 43 FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD MHB LCS MB LAB_ID SAMPLEIO 2185 2186 2187 2188 2189 2190 2191 2192 2193 2194 2195 2196 2197 2198 2199 2200 2201 2202 2203 2381 2383 2447 LF16D1CR PL16L1CR LF16L1CR PL16DOCR LF16DOCR PL16LOCR LF16LOCR PL17D2CR LF17D2CR PL17L2CR LF17L2CR PL18D2CR LF18D2CR PL18L2CR LF18L2CR PL19D2CR LF19D2CR PL19L2CR LF19L2CR MNB LCS MB vuyuons. SUBSTRAT LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX CLMIX 16 16 16 16 16 16 16 17 17 17 17 18 18 18 18 19 19 19 19 SOILTYPE SOILBTCH SMPLTYPE MIL C AMOUNT SRMREC D L L D D L L D D L L D D L L D D L I 1 1 1 0 0 0 0 2 2 2 2 2 2 2 2 2 2 2 2 CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 3.82 2.57 4.67 1.47 2.43 2.62 1.88 2.62 4.89 2.86 9.20 1.74 6.32 2.02 5.87 6.22 4.27 2.56 5.14 1.44 95.50 95 0.32 5 ------- FIELD AND QC LABORATORY DATA 15 CO i—i ON DBS MATRIX 559 SPONGE 560 SPONGE 561 SPONGE 562 SPONGE 563 SPONGE 564 SPONGE 565 SPONGE 566 SPONGE 567 SPONGE 568 SPONGE 569 SPONGE 570 SPONGE 571 SPONGE INSTRMNT GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA PREPBTCH 4816-23 4816-23 4816-23 4816-23 4816-23 4816-23 4816-34 4816-34 4816-34 4816-34 4816-34 4816-34 4816-34 RUN_NO 12 13 14 16 17 20 22 23 24 26 27 28 32 QCJD FIELD FIELD FIELD MMB LCS NB FIELD FIELD FIELD MMB SRM 2710 SRM 2710 MB LABJD 2053 2054 2055 2408 2416 2445 2120 2121 2122 2410 2411 2414 2453 •- IFILE=\ SAMPLEID LF16DOSP PL16LOSP LF16LOSP MMB LCS MB PL32DOSP LF32DOSP PL32LOSP MMB SRM 2710 SRM 2710 MB royotsre.Fi SUBSTRAT LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL i CLMIX 16 16 16 32 32 32 SOILTYPE D L L D D L SOILBTCH 0 0 0 0 0 0 SMPLTYPE SP SP SP SP SP SP MIL 4 2 4 2 4 2 C AMOUNT 2.70 3.23 15.39 25.10 107.75 0.50 1.62 4.73 12.44 2.20 4520.00 4700.00 < 0.19 SRMREC • . » ,, 107.750 . • . . . 81.047 84.517 • ------- FIELD AND QC LABORATORY DATA 16 I I—* *4 OBS 572 573 574 575 576 577 578 579 580 581 582 583 584 585 586 587 588 589 590 591 592 593 594 595 596 597 598 599 600 601 602 603 604 MATRIX WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE INSTRMNT PREPBTCH GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-13 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-8A 4816-13 RUN_NO QCJD 12 13 14 17 18 20 21 24 25 26 28 31 32 33 37 38 39 40 43 47 48 49 52 53 55 56 57 69 70 72 73 74 75 FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD LCS MB FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD LCS MMB MB MMB LABJD SAMPLE ID 2310 2312 2314 2315 2316 2317 2318 2319 2320 2321 2322 2323 2324 2325 2435 2436 2260 2261 2262 2264 2266 2268 2270 2272 2274 2276 2277 2278 2279 2384 2385 2420 2389 PL27D2WW PL27L2WW PL28D2WW LF28D2WW PL28L2WW LF28L2WW PL30D2WW LF30D2WW PL30L2WW LF30L2WW PL32D2WW LF32D2WW PL32L2WW LF32L2WW LCS MB PL01D1WW LF01D1WW PL01L1WW PL03D1WU PL03L1WW PL05D1WW PL05L1WW PL06D1WW PL06L1WW PL11D1WW LF11D1WW PL11L1WW LF11L1WW LCS MMB MB MMB vuyuy/*. SUBSTRAT ENAMEL ENAMEL ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL ENAMEL ENAMEL ENAMEL ENAMEL ENAMEL ENAMEL ENAMEL LATEX ENAMEL LATEX M CLMIX 27 27 28 28 28 28 30 30 30 30 32 32 32 32 01 01 01 03 03 05 05 06 06 11 11 11 11 SOILTYPE SOILBTCH SMPLTYPE MIL C AMOUNT SRMREC D L D D L L D D L L D D L L D D L D L D L D L D D L L 2 2 2 2 2 2 2 2 2 2 2 2 2 2 1 1 1 1 1 1 1 1 1 1 1 1 1 WW WW ww ww ww ww ww ww ww ww ww ww ww ww ww ww ww ww ww ww ww ww ww ww ww ww ww 2 2 2 4 2 4 2 4 2 4 2 4 2 4 4 2 4 2 2 2 2 2 2 2 2 4 2 4 4 17.43 29.87 2.03 19.86 12.02 42.06 4.22 25.69 14.81 25.70 2.05 19.61 3.52 19.32 87.25 87 e 0.19 12.84 39.49 30.42 13.85 39.46 7.14 23.53 6.09 15.83 2.39 45.65 7.73 31.69 99.75 99 0.37 : 0.19 2.12 25 75 ------- FIELD AND QC LABORATORY DATA 17 W >—* 00 OBS MATRIX 605 606 607 608 609 610 611 612 613 614 615 616 617 618 619 620 621 622 623 624 625 626 627 628 629 630 631 632 633 634 635 636 637 638 639 640 641 642 WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE WIPE 1NSTRMNT PREPBTCH RUN_NO QCJD GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-8B 4816-17 4816-17 4816-17 4816-17 4816-17 4816-17 4816-12 4816-12 4816-12 4816-12 4816-12 4816-12 4816-12 4816-12 4816-12 4816-12 4816-12 4816-12 4816-12 4816-12 12 13 14 15 18 19 21 22 23 26 27 28 30 31 32 33 34 35 39 40 41 44 45 46 48 51 52 53 54 57 59 60 61 64 65 66 68 69 FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD LCS MHB MB FIELD FIELD FIELD MMB MB LCS FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD LCS MMB MB LABJD 2280 2282 2283 2284 2285 2286 2288 2289 2290 2292 2293 2294 2296 2326 2327 2386 2387 2421 2331 2346 2361 2439 2440 2441 2298 2299 2300 2302 2304 2305 2306 2307 2308 2398 2399 2388 2433 2434 --- IFILE=V SAMPLE ID PL12D1WW PL12L1VM LF12L1WW PL14D1WW LF14D1WW PL14L1WW PL16D1WW LF16D1WW PL16L1WW PL16DOWW LF16DOWW PL19D2WW PL19L2WW PL32LOWW LF32LOWW LCS MMB MB PCPLL1W2 PCPLD1W2 PCPLL2W2 MMB MB LCS PL21D2WW LF21D2WW PL21L2WW PL22D2WW PL22L2WW LF22L2WW PL26D2WW LF26D2WW PL26L2WW LF12D1WW2 LF12L1WW2 LCS MMB MB OVUV7A.F< SUBSTRAT ENAMEL ENAMEL LATEX ENAMEL LATEX ENAMEL ENAMEL LATEX ENAMEL ENAMEL LATEX ENAMEL ENAMEL ENAMEL LATEX ENAMEL ENAMEL ENAMEL ENAMEL LATEX ENAMEL ENAMEL ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX LATEX i CLMIX 12 12 12 14 14 14 16 16 16 16 16 19 19 32 32 21 21 21 22 22 22 26 26 26 12 12 SOILTYPE SOILBTCH SMPLTYPE MIL C AMOUNT SRMREC D I L D D L D D L D D D L L L L D L D D L D L L D D L D L 1 1 1 1 1 1 1 1 1 0 0 2 2 0 0 1 1 2 2 2 2 2 2 2 2 2 2 1 1 WW WW WW WW WW WW WW WW WW WW WW WW WW WW WW W2 W2 W2 WW WW WW WW WW WW WW WW WW WW2 WW2 2 2 4 2 4 2 2 4 2 2 4 2 2 2 4 2 2 2 2 4 2 2 2 4 2 4 2 4 4 5.31 12.61 21.69 3.64 20.38 7.99 14.02 20.99 13.48 2.45 0.41 5.66 7.02 0.55 0.39 86.50 86 0.34 0.24 14.43 21.12 34.47 2.47 26.81 0.21 0 14.09 27.77 27.56 4.07 9.63 23.85 3.14 25.80 9.25 21.81 15.25 97.00 97 1.02 0.58 50 21 00 ------- FIELD AND QC LABORATORY DATA 18 CO i—> VO DBS MATRIX 643 CORE 644 CORE 645 CORE 646 CORE 647 CORE 648 CORE 649 CORE 650 CORE 651 CORE 652 CORE 653 CORE 654 CORE 655 CORE 656 CORE 657 CORE 658 CORE 659 CORE 660 CORE 661 CORE 662 CORE 663 CORE 664 CORE 665 CORE 666 CORE 667 CORE 668 CORE 669 CORE 670 CORE 671 CORE 672 CORE 673 CORE 674 CORE 675 CORE 676 CORE 677 CORE 678 CORE 679 CORE 680 CORE 681 CORE 682 CORE 683 CORE 684 CORE 685 CORE 686 CORE 687 CORE 688 CORE INSTRMNT GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA PREPBTCH 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-26 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 RUN_ 12 13 14 15 16 29 31 32 33 34 35 36 40 41 42 43 44 45 49 50 51 52 53 56 58 59 60 61 62 63 67 68 69 70 71 72 74 75 88 89 90 91 92 95 96 97 JMLt= NO QC_ID LAB_ID SAMPLE ID FIELD 2204 PL20D2CR FIELD 2205 LF20D2CR FIELD 2206 PL20L2CR FIELD 2207 LF20L2CR FIELD 2208 PL21D2CR FIELD 2209 LF21D2CR FIELD 2210 PL21L2CR FIELD 2211 LF21L2CR FIELD 2212 PL22D2CR FIELD 2213 LF22D2CR FIELD 2214 PL22L2CR FIELD 2215 LF22L2CR FIELD 2216 PL23D2CR FIELD 2217 LF23D2CR FIELD 2218 PL23L2CR FIELD 2219 LF23L2CR FIELD 2220 PL24D2CR FIELD 2221 LF24D2CR FIELD 2222 PL24L2CR FIELD 2223 LF24L2CR LCS 2391 LCS MMB 2395 MMB MB 2448 MB FIELD 2224 PL25D2CR FIELD 2225 LF25D2CR FIELD 2226 PL25L2CR FIELD 2227 LF25L2CR FIELD 2228 PL26D2CR FIELD 2229 LF26D2CR FIELD 2230 PL26L2CR FIELD 2231 LF26L2CR FIELD 2232 PL27D2CR FIELD 2233 LF27D2CR FIELD 2234 PL27L2CR FIELD 2235 LF27L2CR FIELD 2236 PL28D2CR FIELD 2237 LF28D2CR FIELD 2238 PL28L2CR FIELD 2239 LF28L2CR FIELD 2240 PL29D2CR FIELD 2241 LF29D2CR FIELD 2242 PL29L2CR FIELD 2243 LF29L2CR LCS 2397 LCS MMB 2425 MMB MB 2450 MB =vuyiura.i SUBSTRAT ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX M CLMIX 20 20 20 20 21 21 21 21 22 22 22 22 23 23 23 23 24 24 24 24 25 25 25 25 26 26 26 26 27 27 27 27 28 28 28 28 29 29 29 29 SOILTYPE D D L L D D L L D D L L D D L L D D I L D D L L D D L L D D L L D D L L D D L I SOILBTCH 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 SMPLTYPE CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR MIL 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 C AMOUNT SRMREC 1.62 4.23 4.62 2.41 11.92 3.73 2.69 5.66 2.14 2.88 2.66 3.27 2.80 3.90 10.38 6.88 1.93 3.52 5.81 3.97 99.00 99.00 2.90 2.08 2.79 3.98 2.75 3.99 2.75 7.22 2.79 3.32 2.01 3.67 3.36 7.10 3.81 3.50 1.98 6.97 2.50 12.28 6.84 9.84 72.25 72.25 7.41 1.65 ------- FIELD AND QC LABORATORY DATA 19 CD DBS MATRIX 689 690 691 692 693 694 695 696 697 698 699 700 701 702 703 704 705 706 707 708 709 710 711 712 713 714 715 716 717 718 719 720 721 722 723 CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE CORE INSTRMNT PREPBTCH GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA GFAA 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-30 4816-32 4816-32 4816-32 4816-32 4816-32 4816-32 4816-32 4816-37 4816-37 4816-37 4816-37 4816-37 RUN_NO QCJD 12 13 14 15 16 17 21 22 23 24 25 26 30 31 32 33 34 35 39 40 41 42 43 44 48 49 50 51 52 53 55 58 59 60 61 FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD FIELD LCS HMB MB FIELD FIELD FIELD FIELD LCS MMB MB FIELD FIELD LCS MMB MB LABJD 2244 2245 2246 2247 2248 2249 2250 2251 2252 2253 2254 2255 2256 2257 2258 2259 2332 2337 2342 2347 2390 2423 2451 2352 2357 2362 2367 2377 2422 2452 2329 2359 2455 2456 2457 --- IFILE= SAMPLEID PL30D2CR LF30D2CR PL30L2CR LF30L2CR PL31D2CR LF31D2CR PL31L2CR LF31L2CR PL32D2CR LF32D2CR PL32L2CR LF32L2CR PL32DOCR LF32DOCR PL32LOCR LF32LOCR PCPLL1CR PCLFL1CR PCLFD1CR PCPLD1CR LCS MMB MB PCLFD2CR PCPLD2CR PCPLL2CR PCLFL2CR LCS MMB MB PCPLL1RR PCPLL2RR LCS MMB MB V091Q/A. SUBSTRAT ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX ENAMEL LATEX LATEX ENAMEL LATEX ENAMEL ENAMEL LATEX ENAMEL ENAMEL r«J CLMIX 30 30 30 30 31 31 31 31 32 32 32 32 32 32 32 32 SOILTYPE SOILBTCH SMPLTYPE MIL D D L L D D I L D D L L D D L L L L D D D D I L L L 2 2 2 2 2 2 2 2 2 2 2 2 0 0 0 0 1 1 1 1 2 2 2 2 1 2 CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR RR RR 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 2 4 4 2 4 2 2 4 2 2 C AMOUNT SRMREC 3.430 4.960 2.990 3.760 3.560 5.040 2.200 6.900 3.660 4.620 5.330 3.940 5.150 2.720 3.930 2.870 3.570 5.760 6.460 4.160 80.250 80 4.440 3.120 4.940 2.720 3.390 5.420 77.500 77 7.120 1.990 19.650 19.025 93.750 93 0.880 0.290 25 50 75 ------- REPORT DOCUMENTATION PAGE Form Approved OMB No 0704-0188 Public reporting burden for this collection of information is estimated to average 1 hour per response, including the time for reviewing instructions, searching existing data sources, gathering and maintaining the data needed, and completing and reviewing the collection of information. Send comments regarding this burden estimate or any other aspect of this collection of information, including suggestions for reducing this burden, to Washington Headquarters Services, Directorate for Information Operations and Reports, 1215 Jefferson Davis Highway, Suite 1204, Arlington, VA 22202-4302, and to the Office of Management and Budget, Paperwork Reduction Project (0704-0188X Washington, DC 20503. 1. AGENCY USE ONLY (Leave blank) 2. REPORT DATE October 1998 3. REPORT TYPE AND DATES COVERED Final Technical Report 4. TITLE AND SUBTITLE Lead-Cleaning Efficacy Follow-Up Study 6. AUTHOR(s) KarinM Bauer and Gary R. Cooper 5. FUNDING NUMBERS EPA 68-W6-0048 7. PERFORMING ORGANIZATION NAME(s) AND ADDRESS(ES) Midwest Research Institute 425 Volker Boulevard Kansas City, Missouri 64110 8. PERFORMING ORGANIZATION REPORT NUMBER 4701-13 9. SPONSORING/MONITORING AGENCY NAME(S) AND ADDRESS(ES) U.S. Environmental Protection Agency Office of Pollution Prevention and Toxics National Program Chemicals Division 401 M Street, S.W. Washington, D.C. 20460 10. SPONSORING/MONITORING AGENCY REPORT NUMBER EPA747-R-98-008 11. SUPPLEMENTARY NOTES 12.a DISTRIBUTION/AVAILABILITY STATEMENT 12b. DISTRIBUTION CODE 13. ABSTRACT (Maximum 200 words) The U.S. Environmental Protection Agency (EPA) has recommended using a general all-purpose cleaner or a cleaner made specifically for lead for weekly cleaning of residential surfaces. EPA also recommends the use of trisodium phosphate (TSP) detergent to clean lead-contaminated dust from surfaces after residential lead hazard control work to achieve post-abatement clearance standards. Because of negative effects of phosphate detergents on aquatic ecosystems, EPA conducted a laboratory study in 1996797 to evaluate the cleaning efficacy of many commercial household cleaners that could be used to remove lead-contaminated dust from residential surfaces. The study results suggested that low surface tension cleaners remove marginally more lead dust than high surface tension cleaners. The present study is a follow-up to the previous study. The effect of surface tension and phosphate content on cleaning efficacy was further investigated using a wider range of these parameters and a single household cleaner. Surfaces soiled with lead-containing soil were cleaned with a sponge, then half were wiped with a baby wipe. All cleaned surfaces were cored, and all sponges, wipes, and core samples were analyzed for lead. This study showed that surface tension and phosphate content had no statistically significant effect on residual lead found on the test surfaces. The weak link found in the previous study between these parameters and cleaning efficacy could neither be refuted nor strengthened. 14. SUBJECT TERMS Environmental contaminants, lead, clearance testing, TSP, phosphate content, household cleaners, surface tension, wipe sampling, cleaning efficacy 15. NUMBER OF PAGES 72 16. PRICE CODE 17. SECURITY CLASSIFICATION OF REPORT Unclassified 18. SECURITY CLASSIFICATION OF THIS PAGE Unclassified 19. SECURITY CLASSIFICATION OF ABSTRACT Unclassified 20. LIMITATION OF ABSTRACT None NSN 7540-01-280-5500 Standard Form 298 (Rev 2-89) Prescribed by ANSI Std. Z39-18 298-102 ------- |